#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:49:35 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179349 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/46/4324693.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_4324693
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         'C50 H76 N22 O7 P2'
_chemical_formula_sum            'C50 H76 N22 O7 P2'
_chemical_formula_weight         1159.27
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_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_method           SHELXL-97
_cell_angle_alpha                90.000(5)
_cell_angle_beta                 107.644(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            4
_cell_length_a                   24.580(5)
_cell_length_b                   11.104(5)
_cell_length_c                   22.363(5)
_cell_measurement_temperature    293(2)
_cell_volume                     5817(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15889
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  0.9891
_exptl_absorpt_correction_T_min  0.9829
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_description       block
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.750
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0560
_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)+(0.0932P)²+1.0174P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1621
_reflns_number_gt                4376
_reflns_number_total             5700
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic102415x_si_002_05.cif
_cod_data_source_block           Compound-5
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4324693
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.09594(2) 0.21756(5) 0.53325(3) 0.01614(17) Uani 1 1 d .
O1 O 0.09162(7) -0.34177(14) 0.31634(8) 0.0296(4) Uani 1 1 d .
O2 O -0.23456(6) 0.30932(15) 0.41249(8) 0.0278(4) Uani 1 1 d .
O3 O 0.0000 0.5074(2) 0.2500 0.0291(5) Uani 1 2 d S
O4 O 0.82824(8) 0.1808(2) 0.24124(10) 0.0533(6) Uani 1 1 d .
N1 N 0.11712(7) 0.17855(16) 0.60587(8) 0.0180(4) Uani 1 1 d .
N2 N 0.18876(8) 0.20094(17) 0.69977(8) 0.0210(4) Uani 1 1 d .
N3 N 0.13001(7) 0.36260(16) 0.66251(9) 0.0201(4) Uani 1 1 d .
N4 N 0.13398(7) 0.32946(16) 0.52506(8) 0.0185(4) Uani 1 1 d .
N5 N 0.11803(8) 0.37806(17) 0.41817(9) 0.0253(4) Uani 1 1 d .
N6 N 0.20589(8) 0.40800(17) 0.49139(9) 0.0234(4) Uani 1 1 d .
N7 N 0.02696(7) 0.24701(16) 0.51231(8) 0.0178(4) Uani 1 1 d .
N8 N 0.10362(7) 0.10050(16) 0.49039(8) 0.0178(4) Uani 1 1 d .
N9 N 0.00225(7) 0.08164(15) 0.43966(8) 0.0170(4) Uani 1 1 d .
N10 N -0.06720(7) 0.20871(15) 0.45615(8) 0.0156(4) Uani 1 1 d .
N11 N 0.06626(7) -0.05019(15) 0.41670(8) 0.0163(4) Uani 1 1 d .
C1 C 0.14421(9) 0.24812(19) 0.65388(10) 0.0180(5) Uani 1 1 d .
C2 C 0.22060(10) 0.0996(2) 0.68623(11) 0.0265(5) Uani 1 1 d .
H2A H 0.2107 0.0277 0.7044 0.040 Uiso 1 1 calc R
H2B H 0.2608 0.1146 0.7038 0.040 Uiso 1 1 calc R
H2C H 0.2114 0.0897 0.6416 0.040 Uiso 1 1 calc R
C3 C 0.20260(10) 0.2316(2) 0.76596(11) 0.0283(6) Uani 1 1 d .
H3A H 0.2374 0.2771 0.7785 0.042 Uiso 1 1 calc R
H3B H 0.2073 0.1591 0.7904 0.042 Uiso 1 1 calc R
H3C H 0.1722 0.2787 0.7727 0.042 Uiso 1 1 calc R
C4 C 0.07318(9) 0.4115(2) 0.63301(11) 0.0222(5) Uani 1 1 d .
H4A H 0.0738 0.4612 0.5981 0.033 Uiso 1 1 calc R
H4B H 0.0617 0.4590 0.6630 0.033 Uiso 1 1 calc R
H4C H 0.0466 0.3466 0.6185 0.033 Uiso 1 1 calc R
C5 C 0.17217(10) 0.4531(2) 0.69400(12) 0.0301(6) Uani 1 1 d .
H5A H 0.2099 0.4217 0.7003 0.045 Uiso 1 1 calc R
H5B H 0.1673 0.4728 0.7338 0.045 Uiso 1 1 calc R
H5C H 0.1671 0.5243 0.6685 0.045 Uiso 1 1 calc R
C6 C 0.15134(9) 0.36811(19) 0.47813(10) 0.0188(5) Uani 1 1 d .
C7 C 0.24737(9) 0.3787(2) 0.55173(12) 0.0296(6) Uani 1 1 d .
H7A H 0.2493 0.4437 0.5806 0.044 Uiso 1 1 calc R
H7B H 0.2842 0.3668 0.5462 0.044 Uiso 1 1 calc R
H7C H 0.2358 0.3064 0.5680 0.044 Uiso 1 1 calc R
C8 C 0.22303(11) 0.5092(2) 0.45892(12) 0.0317(6) Uani 1 1 d .
H8A H 0.1906 0.5372 0.4259 0.048 Uiso 1 1 calc R
H8B H 0.2522 0.4831 0.4415 0.048 Uiso 1 1 calc R
H8C H 0.2375 0.5734 0.4882 0.048 Uiso 1 1 calc R
C9 C 0.05598(10) 0.3838(2) 0.40226(12) 0.0328(6) Uani 1 1 d .
H9A H 0.0403 0.3047 0.3916 0.049 Uiso 1 1 calc R
H9B H 0.0412 0.4367 0.3671 0.049 Uiso 1 1 calc R
H9C H 0.0456 0.4137 0.4376 0.049 Uiso 1 1 calc R
C10 C 0.13893(12) 0.3612(3) 0.36424(12) 0.0392(7) Uani 1 1 d .
H10A H 0.1781 0.3358 0.3784 0.059 Uiso 1 1 calc R
H10B H 0.1361 0.4357 0.3418 0.059 Uiso 1 1 calc R
H10C H 0.1164 0.3008 0.3370 0.059 Uiso 1 1 calc R
C11 C -0.00782(8) 0.17806(18) 0.47155(10) 0.0155(4) Uani 1 1 d .
C12 C 0.05770(8) 0.05244(18) 0.45270(9) 0.0157(4) Uani 1 1 d .
C13 C 0.02090(9) -0.10762(19) 0.37482(10) 0.0184(5) Uani 1 1 d .
H13 H -0.0159 -0.0805 0.3703 0.022 Uiso 1 1 calc R
C14 C 0.02825(9) -0.20203(19) 0.34013(11) 0.0202(5) Uani 1 1 d .
H14 H -0.0035 -0.2363 0.3113 0.024 Uiso 1 1 calc R
C15 C 0.08390(9) -0.2512(2) 0.34661(11) 0.0213(5) Uani 1 1 d .
C16 C 0.13001(9) -0.18908(19) 0.39131(11) 0.0203(5) Uani 1 1 d .
H16 H 0.1673 -0.2153 0.3978 0.024 Uiso 1 1 calc R
C17 C 0.12028(9) -0.09358(19) 0.42406(10) 0.0185(5) Uani 1 1 d .
H17 H 0.1512 -0.0559 0.4526 0.022 Uiso 1 1 calc R
C18 C -0.10994(9) 0.13320(19) 0.42179(10) 0.0177(5) Uani 1 1 d .
H18 H -0.1003 0.0589 0.4086 0.021 Uiso 1 1 calc R
C19 C -0.16512(9) 0.16516(19) 0.40706(10) 0.0187(5) Uani 1 1 d .
H19 H -0.1927 0.1116 0.3841 0.022 Uiso 1 1 calc R
C20 C -0.18352(9) 0.2793(2) 0.42536(10) 0.0206(5) Uani 1 1 d .
C21 C -0.13662(9) 0.3553(2) 0.45964(11) 0.0251(5) Uani 1 1 d .
H21 H -0.1446 0.4318 0.4718 0.030 Uiso 1 1 calc R
C22 C -0.08225(9) 0.3192(2) 0.47447(11) 0.0215(5) Uani 1 1 d .
H22 H -0.0537 0.3702 0.4979 0.026 Uiso 1 1 calc R
C23 C 0.89612(16) 0.0340(3) 0.2423(2) 0.0748(12) Uani 1 1 d .
H23A H 0.9051 -0.0159 0.2791 0.112 Uiso 1 1 calc R
H23B H 0.9293 0.0421 0.2285 0.112 Uiso 1 1 calc R
H23C H 0.8658 -0.0022 0.2096 0.112 Uiso 1 1 calc R
C24 C 0.87808(11) 0.1538(3) 0.25730(12) 0.0352(6) Uani 1 1 d .
C25 C 0.92314(13) 0.2360(3) 0.29524(13) 0.0451(7) Uani 1 1 d .
H25A H 0.9441 0.2693 0.2692 0.068 Uiso 1 1 calc R
H25B H 0.9487 0.1919 0.3292 0.068 Uiso 1 1 calc R
H25C H 0.9058 0.3000 0.3119 0.068 Uiso 1 1 calc R
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
N4 P1 N1 107.67(9)
N4 P1 N7 113.58(9)
N1 P1 N7 109.31(9)
N4 P1 N8 111.70(10)
N1 P1 N8 108.29(9)
N7 P1 N8 106.17(9)
C1 N1 P1 126.18(16)
C1 N2 C2 120.18(18)
C1 N2 C3 124.38(19)
C2 N2 C3 114.71(18)
C1 N3 C4 122.76(18)
C1 N3 C5 122.75(18)
C4 N3 C5 113.84(18)
C6 N4 P1 133.28(16)
C6 N5 C9 121.43(19)
C6 N5 C10 123.51(19)
C9 N5 C10 114.07(19)
C6 N6 C7 119.76(19)
C6 N6 C8 123.69(19)
C7 N6 C8 113.78(19)
C11 N7 P1 119.03(15)
C12 N8 P1 117.86(15)
C12 N9 C11 114.39(17)
C22 N10 C18 118.55(17)
C22 N10 C11 118.99(17)
C18 N10 C11 122.43(17)
C17 N11 C13 118.22(17)
C17 N11 C12 120.50(17)
C13 N11 C12 121.28(17)
N1 C1 N3 125.24(19)
N1 C1 N2 118.60(19)
N3 C1 N2 116.12(19)
N4 C6 N5 124.97(19)
N4 C6 N6 117.96(19)
N5 C6 N6 116.94(19)
N7 C11 N9 130.78(19)
N7 C11 N10 115.80(18)
N9 C11 N10 113.41(17)
N8 C12 N9 131.70(19)
N8 C12 N11 116.08(18)
N9 C12 N11 112.22(17)
C14 C13 N11 121.99(19)
C13 C14 C15 121.8(2)
O1 C15 C14 122.9(2)
O1 C15 C16 122.8(2)
C14 C15 C16 114.34(19)
C17 C16 C15 121.41(19)
C16 C17 N11 122.26(19)
C19 C18 N10 121.17(19)
C18 C19 C20 122.79(19)
O2 C20 C19 123.3(2)
O2 C20 C21 123.4(2)
C19 C20 C21 113.22(18)
C22 C21 C20 122.2(2)
C21 C22 N10 122.1(2)
O4 C24 C23 120.4(3)
O4 C24 C25 122.1(3)
C23 C24 C25 117.4(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
P1 N4 1.5987(19)
P1 N1 1.6073(19)
P1 N7 1.6492(18)
P1 N8 1.6594(19)
O1 C15 1.258(3)
O2 C20 1.245(3)
O4 C24 1.205(3)
N1 C1 1.327(3)
N2 C1 1.358(3)
N2 C2 1.454(3)
N2 C3 1.455(3)
N3 C1 1.348(3)
N3 C4 1.457(3)
N3 C5 1.462(3)
N4 C6 1.319(3)
N5 C6 1.347(3)
N5 C9 1.459(3)
N5 C10 1.459(3)
N6 C6 1.357(3)
N6 C7 1.460(3)
N6 C8 1.467(3)
N7 C11 1.294(3)
N8 C12 1.301(3)
N9 C12 1.344(3)
N9 C11 1.350(3)
N10 C22 1.379(3)
N10 C18 1.381(3)
N10 C11 1.435(3)
N11 C17 1.375(3)
N11 C13 1.376(3)
N11 C12 1.447(3)
C13 C14 1.348(3)
C14 C15 1.439(3)
C15 C16 1.440(3)
C16 C17 1.351(3)
C18 C19 1.343(3)
C19 C20 1.445(3)
C20 C21 1.447(3)
C21 C22 1.337(3)
C23 C24 1.472(4)
C24 C25 1.487(4)
