#------------------------------------------------------------------------------
#$Date: 2016-03-23 14:49:35 +0100 (Wed 23 de Mar de 2016) $
#$Revision: 179349 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/46/4324697.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4324697
loop_
_publ_author_name
'Vadapalli Chandrasekhar'
'Venkatasubbiah Krishnan'
'Ramachandran Azhakar'
'Tapas Senapati'
'Atanu Dey'
'R. Suriya Narayanan'
_publ_contact_author_address
;Head, Department of Chemistry
Indian Institute of Technology Kanpur
Kanpur 208016
Uttarpradesh
India
;
_publ_contact_author_email       vc@iitk.ac.in
_publ_contact_author_fax         '+91-512-259 7436'
_publ_contact_author_name        'Prof. V. Chandrasekhar'
_publ_contact_author_phone       '+91-512-259 7259'
_publ_section_title
;
 Carbophosphazene-Supported Ligand Systems Containing Pyrazole/Guanidine
 Coordinating Groups
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2568
_journal_page_last               2579
_journal_paper_doi               10.1021/ic102415x
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C31 H30 N14 O3 P2'
_chemical_formula_sum            'C31 H30 N14 O3 P2'
_chemical_formula_weight         708.63
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yac'
_symmetry_space_group_name_H-M   'P 1 2/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 110.904(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.914(4)
_cell_length_b                   11.094(3)
_cell_length_c                   12.800(4)
_cell_measurement_temperature    298(2)
_cell_volume                     1580.5(8)
_computing_cell_refinement       'Bruker SMART V5.628'
_computing_data_collection       'Bruker SMART V5.628'
_computing_data_reduction        'Bruker SAINT+ V6.45'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL 6.14'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.977
_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_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0313
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10238
_diffrn_reflns_theta_full        28.48
_diffrn_reflns_theta_max         28.48
_diffrn_reflns_theta_min         2.50
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_description       plate
_exptl_crystal_F_000             622
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .15
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.607
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3913
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.0777
_refine_ls_R_factor_gt           0.0667
_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/[σ²(Fo²)+(0.1158P)²+0.6014P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1881
_refine_ls_wR_factor_ref         0.1988
_reflns_number_gt                3218
_reflns_number_total             3913
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102415x_si_002_09.cif
_cod_data_source_block           compound-9
_cod_database_code               4324697
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
P1 P 0.15389(5) 0.53514(5) 0.13554(5) 0.0362(2) Uani 1 1 d .
O1 O 0.04910(17) 0.61321(18) 0.10332(16) 0.0535(5) Uani 1 1 d .
O2 O 0.2500 0.5821(2) 0.2500 0.0492(6) Uani 1 2 d S
N1 N 0.12778(18) 0.39378(18) 0.15874(16) 0.0392(4) Uani 1 1 d .
N2 N 0.22025(18) 0.32652(18) 0.03452(16) 0.0377(4) Uani 1 1 d .
N3 N 0.2295(2) 0.53781(17) 0.05026(17) 0.0411(5) Uani 1 1 d .
N4 N 0.13675(18) 0.18941(18) 0.11908(16) 0.0395(4) Uani 1 1 d .
N5 N 0.1860(2) 0.10300(19) 0.07166(19) 0.0458(5) Uani 1 1 d .
N6 N 0.31508(18) 0.43597(18) -0.06218(17) 0.0391(4) Uani 1 1 d .
N7 N 0.3428(2) 0.3250(2) -0.09573(18) 0.0469(5) Uani 1 1 d .
C1 C 0.15953(19) 0.3105(2) 0.10581(18) 0.0343(5) Uani 1 1 d .
C2 C 0.2518(2) 0.4389(2) 0.01046(17) 0.0347(5) Uani 1 1 d .
C3 C 0.0047(3) 0.2070(3) 0.2362(3) 0.0716(9) Uani 1 1 d .
H3A H -0.0414 0.1524 0.2631 0.107 Uiso 1 1 calc R
H3B H -0.0481 0.2637 0.1856 0.107 Uiso 1 1 calc R
H3C H 0.0610 0.2494 0.2983 0.107 Uiso 1 1 calc R
C4 C 0.0706(2) 0.1382(3) 0.1772(2) 0.0491(6) Uani 1 1 d .
C5 C 0.0797(3) 0.0181(3) 0.1650(3) 0.0584(7) Uani 1 1 d .
H5 H 0.0447 -0.0418 0.1942 0.070 Uiso 1 1 calc R
C6 C 0.1516(3) 0.0002(3) 0.1002(2) 0.0516(6) Uani 1 1 d .
C7 C 0.1898(4) -0.1176(3) 0.0680(4) 0.0761(10) Uani 1 1 d .
H7A H 0.2198 -0.1054 0.0084 0.114 Uiso 1 1 calc R
H7B H 0.1223 -0.1714 0.0434 0.114 Uiso 1 1 calc R
H7C H 0.2520 -0.1518 0.1313 0.114 Uiso 1 1 calc R
C8 C 0.3404(3) 0.6590(3) -0.0905(3) 0.0585(7) Uani 1 1 d .
H8A H 0.3848 0.7067 -0.1251 0.088 Uiso 1 1 calc R
H8B H 0.3688 0.6755 -0.0118 0.088 Uiso 1 1 calc R
H8C H 0.2566 0.6788 -0.1230 0.088 Uiso 1 1 calc R
C9 C 0.3574(2) 0.5299(2) -0.1087(2) 0.0421(5) Uani 1 1 d .
C10 C 0.4137(2) 0.4757(3) -0.1725(2) 0.0493(6) Uani 1 1 d .
H10 H 0.4523 0.5143 -0.2147 0.059 Uiso 1 1 calc R
C11 C 0.4024(2) 0.3509(3) -0.1623(2) 0.0478(6) Uani 1 1 d .
C12 C 0.4479(3) 0.2529(3) -0.2162(3) 0.0669(9) Uani 1 1 d .
H12A H 0.5218 0.2219 -0.1638 0.100 Uiso 1 1 calc R
H12B H 0.4618 0.2843 -0.2804 0.100 Uiso 1 1 calc R
H12C H 0.3896 0.1893 -0.2390 0.100 Uiso 1 1 calc R
C13 C 0.2500 0.9829(14) 0.7500 0.199(5) Uiso 1 2 d S
C14 C 0.2965(4) 0.9871(4) 0.8496(4) 0.0828(11) Uiso 1 1 d .
C15 C 0.4182(10) 1.0003(9) 0.9579(10) 0.181(4) Uiso 1 1 d .
C16 C 0.4575(6) 1.0232(5) 1.0118(6) 0.1025(16) Uiso 1 1 d .
H2 H 0.236(3) 0.267(3) 0.002(2) 0.048(8) Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O1 P1 O2 109.23(11) . .
O1 P1 N3 114.81(11) . .
O2 P1 N3 102.74(9) . .
O1 P1 N1 114.86(12) . .
O2 P1 N1 105.42(11) . .
N3 P1 N1 108.68(10) . .
P1 O2 P1 141.79(17) 2 .
C1 N1 P1 118.78(17) . .
C1 N2 C2 121.52(19) . .
C2 N3 P1 119.35(17) . .
N5 N4 C4 111.4(2) . .
N5 N4 C1 119.1(2) . .
C4 N4 C1 129.4(2) . .
C6 N5 N4 105.0(2) . .
C9 N6 N7 111.95(19) . .
C9 N6 C2 129.7(2) . .
N7 N6 C2 118.39(19) . .
C11 N7 N6 104.5(2) . .
N1 C1 N2 126.0(2) . .
N1 C1 N4 121.6(2) . .
N2 C1 N4 112.34(19) . .
N3 C2 N2 125.5(2) . .
N3 C2 N6 121.7(2) . .
N2 C2 N6 112.74(19) . .
C5 C4 N4 105.0(3) . .
C5 C4 C3 130.2(3) . .
N4 C4 C3 124.7(3) . .
C4 C5 C6 107.4(3) . .
N5 C6 C5 111.1(3) . .
N5 C6 C7 122.0(3) . .
C5 C6 C7 126.8(3) . .
C10 C9 N6 104.9(2) . .
C10 C9 C8 130.1(2) . .
N6 C9 C8 125.0(2) . .
C9 C10 C11 107.2(2) . .
N7 C11 C10 111.5(2) . .
N7 C11 C12 120.5(3) . .
C10 C11 C12 128.0(3) . .
C14 C13 C14 175.5(15) 2_556 .
C13 C14 C15 148.3(5) . .
C16 C15 C16 63.1(12) . 3_677
C16 C15 C14 157.2(15) . .
C16 C15 C14 138.6(9) 3_677 .
C16 C15 C15 42.7(9) . 3_677
C16 C15 C15 20.4(4) 3_677 3_677
C14 C15 C15 158.5(11) . 3_677
C15 C16 C16 86.1(12) . 3_677
C15 C16 C15 116.9(12) . 3_677
C16 C16 C15 30.9(5) 3_677 3_677
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 O1 1.4531(19) .
P1 O2 1.5910(10) .
P1 N3 1.645(2) .
P1 N1 1.646(2) .
O2 P1 1.5910(10) 2
N1 C1 1.280(3) .
N2 C1 1.363(3) .
N2 C2 1.369(3) .
N3 C2 1.277(3) .
N4 N5 1.373(3) .
N4 C4 1.384(3) .
N4 C1 1.393(3) .
N5 C6 1.307(4) .
N6 C9 1.381(3) .
N6 N7 1.382(3) .
N6 C2 1.391(3) .
N7 C11 1.321(3) .
C3 C4 1.481(4) .
C4 C5 1.350(4) .
C5 C6 1.403(5) .
C6 C7 1.490(4) .
C8 C9 1.476(4) .
C9 C10 1.368(4) .
C10 C11 1.401(4) .
C11 C12 1.490(4) .
C13 C14 1.196(4) 2_556
C13 C14 1.196(4) .
C14 C15 1.615(12) .
C15 C16 0.728(11) .
C15 C16 1.415(10) 3_677
C15 C15 1.86(2) 3_677
C16 C16 1.264(11) 3_677
C16 C15 1.415(10) 3_677
