Metalation studies of 3- and 4-pyridyloxycyclophosphazenes: metallamacrocycles to coordination polymers.
Chandrasekhar, Vadapalli; Narayanan, Ramakirushnan Suriya; Dalton transactions (Cambridge, England : 2003) 42 (2013) 6619–6632; doi:10.1039/c3dt33084b

data_7022818
_publ_section_title
;
 Metalation studies of 3- and 4-pyridyloxycyclophosphazenes:
 metallamacrocycles to coordination polymers.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6619
_journal_page_last               6632
_journal_paper_doi               10.1039/c3dt33084b
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C32 H24 N7 O6 P3'
_chemical_formula_sum            'C32 H24 N7 O6 P3'
_chemical_formula_weight         695.49
_chemical_name_common            spiro(tetrakis-3-pyridyloxy)cyclotriphosphazene
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-02-05
_audit_creation_method
;
Olex2 1.2
(compiled Dec 5 2012 16:20:19, GUI svn.r4385)
;
_cell_angle_alpha                76.683(2)
_cell_angle_beta                 82.873(2)
_cell_angle_gamma                88.340(2)
_cell_formula_units_Z            4
_cell_length_a                   11.6031(15)
_cell_length_b                   14.6279(19)
_cell_length_c                   19.142(3)
_cell_measurement_reflns_used    2666
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.48
_cell_measurement_theta_min      2.19
_cell_volume                     3137.2(8)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0469
_diffrn_reflns_av_unetI/netI     0.0986
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17656
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.19
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.608419
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0781 before and 0.0374 after correction.
The Ratio of minimum to maximum transmission is 0.6084.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.398
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     865
_refine_ls_number_reflns         12046
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0966
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1293
_refine_ls_wR_factor_ref         0.1554
_reflns_number_gt                7914
_reflns_number_total             12046
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt33084b.txt
_cod_data_source_block           908589
_cod_original_cell_volume        3137.1(7)
_cod_database_code               7022818
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
H2BP of C2BP, H5BP of C5BP, H4BP of C4BP, H3BP of C3BP, H8BP of C8BP, H9BP
of C9BP, H10B of C10B, H11B of C11B, H2D of C2D, H5C of C5C, H2C of C2C, H2A
of C2A, H4C of C4C, H4B of C4B, H3A of C3A, H5A of C5A, H3C of C3C, H2B of
C2B, H5B of C5B, H4A of C4A, H3B of C3B, H11D of C11D, H3X of C3X, H5W of C5W,
H2W of C2W, H3W of C3W, H4W of C4W, H5X of C5X, H2Y of C2Y, H3Y of C3Y, H4Y
of C4Y, H5Y of C5Y, H4X of C4X, H2X of C2X, H4Z of C4Z, H3Z of C3Z, H2Z of
C2Z, H5Z of C5Z, H3D of C3D, H4D of C4D, H5D of C5D, H2DP of C2DP, H5DP of
C5DP, H8DP of C8DP, H10D of C10D, H4DP of C4DP, H9DP of C9DP, H3DP of C3DP
2.a Aromatic/amide H refined with riding coordinates:
C2BP(H2BP), C3BP(H3BP), C4BP(H4BP), C5BP(H5BP), C8BP(H8BP), C9BP(H9BP),
C10B(H10B), C11B(H11B), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C2B(H2B),
C3B(H3B), C4B(H4B), C5B(H5B), C2C(H2C), C3C(H3C), C4C(H4C), C5C(H5C), C2D(H2D),
C3D(H3D), C4D(H4D), C5D(H5D), C2DP(H2DP), C3DP(H3DP), C4DP(H4DP), C5DP(H5DP),
C8DP(H8DP), C9DP(H9DP), C10D(H10D), C11D(H11D), C2W(H2W), C3W(H3W), C4W(H4W),
C5W(H5W), C2X(H2X), C3X(H3X), C4X(H4X), C5X(H5X), C2Y(H2Y), C3Y(H3Y), C4Y(H4Y),
C5Y(H5Y), C2Z(H2Z), C3Z(H3Z), C4Z(H4Z), C5Z(H5Z)
;