#------------------------------------------------------------------------------
#$Date: 2020-11-05 10:56:28 +0200 (Thu, 05 Nov 2020) $
#$Revision: 258736 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/31/28/4312897.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_4312897
loop_
_publ_author_name
'Vadapalli Chandrasekhar'
'Arunachalampillai Athimoolam'
'Narreddula Dastagiri Reddy'
'Selvarajan Nagendran'
'Alexander Steiner'
'Stefano Zacchini'
'Raymond Butcher'
_publ_section_title
;
 Pendant Cyclodicarbaphosphazatriene-Containing Monomers and Polymers:
 Synthesis, Crystal Structures and Polymerization Behavior of
 [NC(NMe2)]2[NP(O-C6H4-p-C6H4-p-CHCH2)(X)], X = Cl, OCH2CF3, OC6H5,
 OC6H4-m-CH3, OC6H4-p-Br
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              51
_journal_page_last               59
_journal_paper_doi               10.1021/ic025940u
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C26 H27 Br N5 O2 P'
_chemical_formula_weight         552.41
_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                 90.4080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.8123(11)
_cell_length_b                   8.6986(4)
_cell_length_c                   12.6785(6)
_cell_measurement_temperature    150(2)
_cell_volume                     2515.8(2)
_computing_structure_refinement  'shelxl-97 (sheldrick, 1997)'
_computing_structure_solution    'shelxs-97 (sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'bruker axs smart apex'
_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  0.0535
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12690
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.79
_exptl_absorpt_coefficient_mu    1.731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(sadabs, sheldrick 2001)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.594
_refine_diff_density_min         -0.771
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     320
_refine_ls_number_reflns         4409
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0378
_refine_ls_R_factor_gt           0.0334
_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/[σ²(fo²)+(0.0592p)²+0.0000p] where p=(fo²+2fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0892
_reflns_number_gt                3818
_reflns_number_total             4409
_reflns_threshold_expression     >2sigma(i)
_cod_data_source_file            ic025940u-2_s2_5.cif
_cod_data_source_block           compd7
_cod_depositor_comments
;
 Changing the capitalization of '_atom_type_symbol' data item
 values and the values of related data items (e. g. _atom_site_type_symbol).
 Updating the _chemical_formula_sum data item value.

 Antanas Vaitkus,
 2017-01-04

The following automatic conversions were performed:

'_refine_ls_structure_factor_coef' value 'fsqd' changed to 'Fsqd'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

'_atom_site_adp_type'
value 'uani' changed to 'Uani' according to the built-in table from
CIF Core dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29 (35 times).

'_atom_site_adp_type' value 'uiso' changed to
'Uiso' according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (27
times).

'_atom_site_refinement_flags' value 'r' changed to 'R'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (27 times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

2020-11-03
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         736.54
_cod_original_formula_units_Z            3
_cod_original_formula_sum        'c34.67 h36 br1.33 n6.67 o2.67 p1.33'
_cod_database_code               4312897
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
br1 Br 1.037713(10) 0.66623(3) 1.424567(19) 0.04346(11) Uani 1 1 d . . .
c1 C 0.76308(8) 0.3250(2) 1.14502(15) 0.0198(4) Uani 1 1 d . . .
c2 C 0.81939(8) 0.3288(2) 0.99366(15) 0.0196(4) Uani 1 1 d . . .
c3 C 0.70110(9) 0.2971(2) 1.30208(16) 0.0263(4) Uani 1 1 d . . .
h3a H 0.7190 0.2719 1.3686 0.040 Uiso 1 1 calc R . .
h3b H 0.6625 0.2535 1.2987 0.040 Uiso 1 1 calc R . .
h3c H 0.6985 0.4068 1.2951 0.040 Uiso 1 1 calc R . .
c4 C 0.74022(10) 0.0678(2) 1.21084(17) 0.0312(5) Uani 1 1 d . . .
h4a H 0.7057 0.0281 1.1768 0.047 Uiso 1 1 calc R . .
h4b H 0.7433 0.0259 1.2807 0.047 Uiso 1 1 calc R . .
h4c H 0.7742 0.0393 1.1710 0.047 Uiso 1 1 calc R . .
c5 C 0.84015(9) 0.0756(2) 0.91711(16) 0.0276(5) Uani 1 1 d . . .
h5a H 0.8180 0.0423 0.9770 0.041 Uiso 1 1 calc R . .
h5b H 0.8782 0.0287 0.9191 0.041 Uiso 1 1 calc R . .
h5c H 0.8201 0.0458 0.8535 0.041 Uiso 1 1 calc R . .
c6 C 0.88083(9) 0.3100(2) 0.83546(16) 0.0288(5) Uani 1 1 d . . .
h6a H 0.8608 0.2955 0.7693 0.043 Uiso 1 1 calc R . .
h6b H 0.9185 0.2608 0.8330 0.043 Uiso 1 1 calc R . .
h6c H 0.8859 0.4179 0.8483 0.043 Uiso 1 1 calc R . .
c7 C 0.87763(9) 0.6831(2) 1.19731(15) 0.0211(4) Uani 1 1 d . . .
c8 C 0.87701(9) 0.7698(2) 1.28919(15) 0.0244(4) Uani 1 1 d . . .
h8 H 0.8453 0.8331 1.3041 0.029 Uiso 1 1 calc R . .
c9 C 0.92395(9) 0.7611(2) 1.35816(15) 0.0274(5) Uani 1 1 d . . .
h9 H 0.9241 0.8186 1.4200 0.033 Uiso 1 1 calc R . .
c10 C 0.97064(9) 0.6666(2) 1.33463(17) 0.0273(5) Uani 1 1 d . . .
c11 C 0.97042(9) 0.5762(2) 1.24498(17) 0.0287(5) Uani 1 1 d . . .
h11 H 1.0016 0.5101 1.2317 0.034 Uiso 1 1 calc R . .
c12 C 0.92346(9) 0.5845(2) 1.17461(16) 0.0267(4) Uani 1 1 d . . .
h12 H 0.9229 0.5251 1.1136 0.032 Uiso 1 1 calc R . .
c13 C 0.70606(9) 0.6777(2) 0.94718(15) 0.0213(4) Uani 1 1 d . . .
c14 C 0.70367(9) 0.7754(2) 0.86071(16) 0.0240(4) Uani 1 1 d . . .
h14 H 0.7326 0.8494 0.8512 0.029 Uiso 1 1 calc R . .
c15 C 0.65840(9) 0.7622(2) 0.78927(15) 0.0235(4) Uani 1 1 d . . .
h15 H 0.6572 0.8283 0.7316 0.028 Uiso 1 1 calc R . .
c16 C 0.61380(8) 0.6516(2) 0.80068(15) 0.0210(4) Uani 1 1 d . . .
c17 C 0.61912(8) 0.5518(2) 0.88669(15) 0.0231(4) Uani 1 1 d . . .
h17 H 0.5914 0.4745 0.8949 0.028 Uiso 1 1 calc R . .
c18 C 0.66433(9) 0.5641(2) 0.96039(15) 0.0227(4) Uani 1 1 d . . .
h18 H 0.6665 0.4971 1.0175 0.027 Uiso 1 1 calc R . .
c19 C 0.56376(9) 0.6429(2) 0.72547(15) 0.0222(4) Uani 1 1 d . . .
c20 C 0.56484(9) 0.7179(2) 0.62745(16) 0.0281(5) Uani 1 1 d . . .
h20 H 0.5985 0.7707 0.6079 0.034 Uiso 1 1 calc R . .
c21 C 0.51756(9) 0.7155(2) 0.55955(16) 0.0294(5) Uani 1 1 d . . .
h21 H 0.5197 0.7682 0.4959 0.035 Uiso 1 1 calc R . .
c22 C 0.46648(9) 0.6357(2) 0.58415(16) 0.0262(5) Uani 1 1 d . . .
c23 C 0.46574(9) 0.5576(2) 0.67953(17) 0.0321(5) Uani 1 1 d . . .
h23 H 0.4326 0.5014 0.6975 0.039 Uiso 1 1 calc R . .
c24 C 0.51303(9) 0.5610(2) 0.74875(16) 0.0305(5) Uani 1 1 d . . .
h24 H 0.5108 0.5075 0.8121 0.037 Uiso 1 1 calc R . .
c25 C 0.41432(10) 0.6312(3) 0.51422(17) 0.0319(5) Uani 1 1 d . . .
h25 H 0.3846 0.5637 0.5332 0.038 Uiso 1 1 calc R . .
c26 C 0.40558(11) 0.7122(3) 0.42828(19) 0.0434(6) Uani 1 1 d . . .
h26a H 0.4340 0.7814 0.4058 0.052 Uiso 1 1 calc R . .
h26b H 0.3710 0.7005 0.3898 0.052 Uiso 1 1 calc R . .
n1 N 0.75944(7) 0.48003(17) 1.15932(12) 0.0218(3) Uani 1 1 d . . .
n2 N 0.79030(7) 0.24970(18) 1.06724(12) 0.0219(4) Uani 1 1 d . . .
n3 N 0.82485(7) 0.48449(17) 0.98529(12) 0.0219(4) Uani 1 1 d . . .
n4 N 0.73640(7) 0.23513(18) 1.21693(12) 0.0230(4) Uani 1 1 d . . .
n5 N 0.84640(7) 0.24294(17) 0.91972(12) 0.0222(4) Uani 1 1 d . . .
o1 O 0.83183(6) 0.70948(14) 1.12593(11) 0.0240(3) Uani 1 1 d . . .
o2 O 0.75002(6) 0.70769(14) 1.02163(11) 0.0240(3) Uani 1 1 d . . .
p1 P 0.79164(2) 0.58117(5) 1.07302(4) 0.01916(13) Uani 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'
Br Br -0.2901 2.4595 '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
_geom_angle_publ_flag
n2 c1 n4 115.32(16) . . ?
n2 c1 n1 127.62(17) . . ?
n4 c1 n1 117.06(17) . . ?
n2 c2 n5 115.50(16) . . ?
n2 c2 n3 127.59(17) . . ?
n5 c2 n3 116.91(17) . . ?
c12 c7 c8 121.56(18) . . ?
c12 c7 o1 122.00(17) . . ?
c8 c7 o1 116.28(17) . . ?
c9 c8 c7 119.34(19) . . ?
c10 c9 c8 119.48(19) . . ?
c9 c10 c11 121.24(19) . . ?
c9 c10 br1 119.35(16) . . ?
c11 c10 br1 119.37(16) . . ?
c10 c11 c12 119.75(19) . . ?
c7 c12 c11 118.57(19) . . ?
c18 c13 c14 120.67(18) . . ?
c18 c13 o2 122.90(17) . . ?
c14 c13 o2 116.30(16) . . ?
c15 c14 c13 119.64(18) . . ?
c14 c15 c16 121.98(18) . . ?
c17 c16 c15 116.44(18) . . ?
c17 c16 c19 122.10(17) . . ?
c15 c16 c19 121.45(17) . . ?
c18 c17 c16 122.44(18) . . ?
c13 c18 c17 118.75(17) . . ?
c24 c19 c20 116.43(18) . . ?
c24 c19 c16 121.79(18) . . ?
c20 c19 c16 121.78(18) . . ?
c21 c20 c19 121.89(19) . . ?
c20 c21 c22 121.38(19) . . ?
c23 c22 c21 117.03(19) . . ?
c23 c22 c25 119.64(19) . . ?
c21 c22 c25 123.33(19) . . ?
c24 c23 c22 121.8(2) . . ?
c23 c24 c19 121.42(19) . . ?
c26 c25 c22 126.9(2) . . ?
c1 n1 p1 115.30(13) . . ?
c2 n2 c1 119.75(16) . . ?
c2 n3 p1 115.24(13) . . ?
c1 n4 c3 122.78(16) . . ?
c1 n4 c4 120.96(16) . . ?
c3 n4 c4 116.24(16) . . ?
c2 n5 c6 122.70(16) . . ?
c2 n5 c5 121.39(16) . . ?
c6 n5 c5 115.85(15) . . ?
c7 o1 p1 125.78(12) . . ?
c13 o2 p1 124.83(12) . . ?
n1 p1 o1 111.49(8) . . ?
n1 p1 o2 112.83(8) . . ?
o1 p1 o2 91.60(7) . . ?
n1 p1 n3 114.44(8) . . ?
o1 p1 n3 112.96(8) . . ?
o2 p1 n3 111.43(8) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
br1 c10 1.902(2) . ?
c1 n2 1.340(2) . ?
c1 n4 1.349(2) . ?
c1 n1 1.363(2) . ?
c2 n2 1.339(2) . ?
c2 n5 1.350(2) . ?
c2 n3 1.364(2) . ?
c3 n4 1.455(2) . ?
c4 n4 1.460(2) . ?
c5 n5 1.463(2) . ?
c6 n5 1.453(3) . ?
c7 c12 1.384(3) . ?
c7 c8 1.388(3) . ?
c7 o1 1.396(2) . ?
c8 c9 1.380(3) . ?
c9 c10 1.380(3) . ?
c10 c11 1.382(3) . ?
c11 c12 1.391(3) . ?
c13 c18 1.383(3) . ?
c13 c14 1.388(3) . ?
c13 o2 1.397(2) . ?
c14 c15 1.374(3) . ?
c15 c16 1.408(3) . ?
c16 c17 1.398(3) . ?
c16 c19 1.484(3) . ?
c17 c18 1.391(3) . ?
c19 c24 1.392(3) . ?
c19 c20 1.404(3) . ?
c20 c21 1.375(3) . ?
c21 c22 1.393(3) . ?
c22 c23 1.387(3) . ?
c22 c25 1.479(3) . ?
c23 c24 1.386(3) . ?
c25 c26 1.312(3) . ?
n1 p1 1.5882(16) . ?
n3 p1 1.5907(16) . ?
o1 p1 1.5899(14) . ?
o2 p1 1.5900(14) . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
c12 c7 c8 c9 1.9(3) . . . . ?
o1 c7 c8 c9 -173.44(16) . . . . ?
c7 c8 c9 c10 0.0(3) . . . . ?
c8 c9 c10 c11 -2.2(3) . . . . ?
c8 c9 c10 br1 175.44(15) . . . . ?
c9 c10 c11 c12 2.6(3) . . . . ?
br1 c10 c11 c12 -175.13(15) . . . . ?
c8 c7 c12 c11 -1.6(3) . . . . ?
o1 c7 c12 c11 173.49(17) . . . . ?
c10 c11 c12 c7 -0.6(3) . . . . ?
c18 c13 c14 c15 2.0(3) . . . . ?
o2 c13 c14 c15 -173.95(17) . . . . ?
c13 c14 c15 c16 -0.1(3) . . . . ?
c14 c15 c16 c17 -2.3(3) . . . . ?
c14 c15 c16 c19 177.33(18) . . . . ?
c15 c16 c17 c18 2.8(3) . . . . ?
c19 c16 c17 c18 -176.79(17) . . . . ?
c14 c13 c18 c17 -1.5(3) . . . . ?
o2 c13 c18 c17 174.20(17) . . . . ?
c16 c17 c18 c13 -1.0(3) . . . . ?
c17 c16 c19 c24 15.2(3) . . . . ?
c15 c16 c19 c24 -164.39(18) . . . . ?
c17 c16 c19 c20 -165.44(19) . . . . ?
c15 c16 c19 c20 15.0(3) . . . . ?
c24 c19 c20 c21 2.3(3) . . . . ?
c16 c19 c20 c21 -177.15(19) . . . . ?
c19 c20 c21 c22 -1.2(3) . . . . ?
c20 c21 c22 c23 -0.7(3) . . . . ?
c20 c21 c22 c25 179.32(19) . . . . ?
c21 c22 c23 c24 1.4(3) . . . . ?
c25 c22 c23 c24 -178.6(2) . . . . ?
c22 c23 c24 c19 -0.3(3) . . . . ?
c20 c19 c24 c23 -1.5(3) . . . . ?
c16 c19 c24 c23 177.88(19) . . . . ?
c23 c22 c25 c26 171.6(2) . . . . ?
c21 c22 c25 c26 -8.4(4) . . . . ?
n2 c1 n1 p1 -0.2(3) . . . . ?
n4 c1 n1 p1 179.81(13) . . . . ?
n5 c2 n2 c1 178.71(17) . . . . ?
n3 c2 n2 c1 -1.1(3) . . . . ?
n4 c1 n2 c2 -178.20(17) . . . . ?
n1 c1 n2 c2 1.8(3) . . . . ?
n2 c2 n3 p1 -1.0(3) . . . . ?
n5 c2 n3 p1 179.19(13) . . . . ?
n2 c1 n4 c3 -175.25(17) . . . . ?
n1 c1 n4 c3 4.8(3) . . . . ?
n2 c1 n4 c4 2.8(3) . . . . ?
n1 c1 n4 c4 -177.17(17) . . . . ?
n2 c2 n5 c6 -178.75(17) . . . . ?
n3 c2 n5 c6 1.1(3) . . . . ?
n2 c2 n5 c5 4.3(3) . . . . ?
n3 c2 n5 c5 -175.85(16) . . . . ?
c12 c7 o1 p1 54.6(2) . . . . ?
c8 c7 o1 p1 -130.00(16) . . . . ?
c18 c13 o2 p1 49.8(2) . . . . ?
c14 c13 o2 p1 -134.35(15) . . . . ?
c1 n1 p1 o1 -131.59(13) . . . . ?
c1 n1 p1 o2 126.97(13) . . . . ?
c1 n1 p1 n3 -1.84(17) . . . . ?
c7 o1 p1 n1 57.63(17) . . . . ?
c7 o1 p1 o2 172.97(15) . . . . ?
c7 o1 p1 n3 -72.90(16) . . . . ?
c13 o2 p1 n1 -75.22(16) . . . . ?
c13 o2 p1 o1 170.62(15) . . . . ?
c13 o2 p1 n3 55.14(17) . . . . ?
c2 n3 p1 n1 2.34(17) . . . . ?
c2 n3 p1 o1 131.36(13) . . . . ?
c2 n3 p1 o2 -127.17(14) . . . . ?
