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_7022820
_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
'C64 H48 Ag4 N14 O12 P6, 2(C H4 O), 3(N O3), 2(H2 O), 2(C1.5 N O2)'
_chemical_formula_sum            'C69 H60 Ag4 N19 O29 P6'
_chemical_formula_weight         2236.66
_chemical_name_systematic
;
?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_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     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                90.00
_cell_angle_beta                 112.26(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.730(2)
_cell_length_b                   11.791(3)
_cell_length_c                   26.394(4)
_cell_measurement_reflns_used    8096
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.32
_cell_volume                     7987(3)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0565
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            21219
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.32
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.628292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0967 before and 0.0262 after correction.
The Ratio of minimum to maximum transmission is 0.6283.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.860
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4468
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.138
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         7720
_refine_ls_number_restraints     76
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0452
_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^)+(0.0583P)^2^+19.3021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                6579
_reflns_number_total             7720
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt33084b.txt
_cod_data_source_block           908591
_cod_original_cell_volume        7987.0(2)
_cod_database_code               7022820
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
H4 of C4, H3 of C3, H8 of C8, H2 of C2, H5 of C5, H10 of C10, H9 of C9, H11
of C11, H20 of C20, H25 of C25, H16 of C16, H30 of C30, H19 of C19, H27 of
C27, H15 of C15, H31 of C31, H17 of C17, H22 of C22, H24 of C24, H26 of C26,
H29 of C29, H14 of C14, H21 of C21, H32 of C32
At 1.5 times of:
H13 of O13, {H33A,H33B,H33C} of C33, {H12A,H12B} of O12
2. Restrained distances
N10-C34 = N10-C37 = N10-C36 = N10-O15 = N10-O16 = N10-O14
1.24 with sigma of 0.02
N10-C34
1.26 with sigma of 0.02
N10-C34 = N10-C37 = N10-C36 = N10-O15 = N10-O16 = N10-O14
1.26 with sigma of 0.02
O18-C36
1.46 with sigma of 0.02
N10-C34 = N10-C37 = N10-C36 = N10-O15 = N10-O16 = N10-O14
1.26 with sigma of 0.02
N10-C34
1.26 with sigma of 0.02
N10-C34
1.26 with sigma of 0.02
N10-C34
1.26 with sigma of 0.02
N10-C34
1.26 with sigma of 0.02
O18-C36
1.46 with sigma of 0.02
C34-C37
2.1 with sigma of 0.04
C36-C34
2 with sigma of 0.04
C34-C36
2 with sigma of 0.04
C36-C37
2 with sigma of 0.04
C34-C37
2 with sigma of 0.04
C37-C34
1.8 with sigma of 0.04
C37-C34
1.8 with sigma of 0.04
C37-O18
2 with sigma of 0.04
C37-C34
2 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(N10) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O14) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O15) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O16) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C34) ~ Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C36) = Uanis(O16)
Uanis(C37) = Uanis(O15)
4. Others
Fixed Sof: O7(0.5) O8A(0.5) O8B(0.5) C34(0.5) O18(0.5) C37(0.5) C36(0.5)
O15(0.5) O16(0.5) O14(0.5)
5.a Free rotating group:
O12(H12A,H12B)
5.b Aromatic/amide H refined with riding coordinates:
C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C21(H21), C22(H22), C24(H24),
C25(H25), C26(H26), C27(H27), C29(H29), C30(H30), C31(H31), C32(H32)
5.c Idealised Me refined as rotating group:
C33(H33A,H33B,H33C)
5.d Idealised tetrahedral OH refined as rotating group:
O13(H13)
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