#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:23:38 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180076 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/22/7052226.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_7052226
loop_
_publ_author_name
'Kumar, K. V. P. Pavan'
'Kumar, N. Satish'
'Kumara Swamy, K. C.'
_publ_section_title
;
 Structurally diverse penta- and hexacoordinate phosphorus compounds
 from the reaction of diethyl or diisopropyl azodicarboxylates with
 phosphorus(iii) compounds
;
_journal_issue                   5
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              717
_journal_paper_doi               10.1039/b514839a
_journal_volume                  30
_journal_year                    2006
_chemical_formula_sum            'C41 H55 N4 O6 P'
_chemical_formula_weight         730.86
_chemical_name_systematic
;
?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.235(3)
_cell_length_b                   18.659(4)
_cell_length_c                   13.113(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4217.0(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_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  0.0615
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26032
_diffrn_reflns_theta_full        28.23
_diffrn_reflns_theta_max         28.23
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_T_max  0.9888
_exptl_absorpt_correction_T_min  0.9669
_exptl_absorpt_correction_type   'EMPIRICAL, SADABS'
_exptl_crystal_colour            COLOURLESS
_exptl_crystal_density_diffrn    1.151
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       NEEDLES
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.191
_refine_diff_density_min         -0.198
_refine_diff_density_rms         0.036
_refine_ls_extinction_coef       0.0019(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     339
_refine_ls_number_reflns         5200
_refine_ls_number_restraints     388
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0822P)²+0.0277P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1640
_reflns_number_gt                2460
_reflns_number_total             5200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b514839a.txt
_cod_data_source_block           compd13b
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'ORTHORHOMBIC' changed to 'orthorhombic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+0.0277P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0822P)^2^+0.0277P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      Pnma
_cod_database_code               7052226
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
P P 0.25458(4) 0.2500 0.56912(5) 0.0574(3) Uani 1 d SU . .
O1 O 0.30299(7) 0.17772(7) 0.57410(8) 0.0551(4) Uani 1 d U . .
O2 O 0.23990(9) 0.2500 0.69967(12) 0.0584(5) Uani 1 d SU . .
C24 C 0.16585(14) 0.2500 0.72376(19) 0.0535(7) Uani 1 d SU . .
N2 N 0.11440(12) 0.2500 0.65404(16) 0.0605(6) Uani 1 d SU . .
N1 N 0.15763(12) 0.2500 0.56120(16) 0.0695(7) Uani 1 d SU . .
O3 O 0.14639(11) 0.2500 0.82059(13) 0.0770(6) Uani 1 d SDU . .
C25 C 0.2070(2) 0.2560(7) 0.8985(3) 0.0729(15) Uani 0.50 d PDU A -1
H25 H 0.2532 0.2790 0.8701 0.087 Uiso 0.50 calc PR A -1
C26 C 0.1753(5) 0.2996(4) 0.9857(4) 0.135(3) Uani 0.50 d PDU A -1
H26A H 0.1669 0.3480 0.9636 0.203 Uiso 0.50 calc PR A -1
H26B H 0.2118 0.2993 1.0411 0.203 Uiso 0.50 calc PR A -1
H26C H 0.1270 0.2793 1.0082 0.203 Uiso 0.50 calc PR A -1
C27 C 0.2246(4) 0.1801(4) 0.9279(5) 0.1078(19) Uani 0.50 d PDU A -1
H27A H 0.2460 0.1552 0.8703 0.162 Uiso 0.50 calc PR A -1
H27B H 0.1778 0.1567 0.9493 0.162 Uiso 0.50 calc PR A -1
H27C H 0.2614 0.1797 0.9828 0.162 Uiso 0.50 calc PR A -1
C28 C 0.1098(2) 0.2153(3) 0.4776(3) 0.0649(11) Uani 0.50 d PU B -1
O4 O 0.12492(19) 0.16499(19) 0.4268(2) 0.0886(10) Uani 0.50 d PU B -1
O5 O 0.04853(14) 0.2500 0.47287(18) 0.1097(9) Uani 1 d SDU . .
C29 C -0.0094(3) 0.2325(8) 0.3932(4) 0.111(5) Uani 0.50 d PDU B -1
H29 H -0.0083 0.1812 0.3774 0.134 Uiso 0.50 calc PR B -1
C30 C 0.0103(4) 0.2751(10) 0.3022(5) 0.226(11) Uani 0.50 d PDU B -1
H30A H 0.0656 0.2764 0.2940 0.339 Uiso 0.50 calc PR B -1
H30B H -0.0090 0.3230 0.3102 0.339 Uiso 0.50 calc PR B -1
H30C H -0.0128 0.2536 0.2430 0.339 Uiso 0.50 calc PR B -1
C31 C -0.0861(3) 0.2531(15) 0.4403(4) 0.207(4) Uani 0.50 d PDU B -1
H31A H -0.0813 0.2534 0.5132 0.311 Uiso 0.50 calc PR B -1
H31B H -0.1251 0.2191 0.4204 0.311 Uiso 0.50 calc PR B -1
H31C H -0.1008 0.3000 0.4171 0.311 Uiso 0.50 calc PR B -1
N3 N 0.26481(12) 0.2500 0.43615(16) 0.0586(6) Uani 1 d SU . .
C32 C 0.3018(3) 0.1955(3) 0.3719(3) 0.0715(12) Uani 0.50 d PU C -1
H32 H 0.3239 0.1532 0.3957 0.086 Uiso 0.50 calc PR C -1
N4 N 0.2989(3) 0.2149(4) 0.2776(6) 0.091(2) Uani 0.50 d PU C -1
C34 C 0.2375(3) 0.2947(3) 0.3730(3) 0.0711(12) Uani 0.50 d PU C -1
H34 H 0.2074 0.3341 0.3906 0.085 Uiso 0.50 calc PR C -1
C33 C 0.2576(4) 0.2777(5) 0.2778(7) 0.082(2) Uani 0.50 d PU C -1
H33 H 0.2455 0.3044 0.2201 0.098 Uiso 0.50 calc PR C -1
C1 C 0.33732(10) 0.14575(11) 0.66112(13) 0.0571(5) Uani 1 d U . .
C2 C 0.31266(11) 0.07838(12) 0.69406(15) 0.0649(5) Uani 1 d U . .
C3 C 0.35033(13) 0.05205(14) 0.77979(17) 0.0801(7) Uani 1 d U . .
H3 H 0.3347 0.0080 0.8058 0.096 Uiso 1 calc R . .
C4 C 0.40999(13) 0.08802(14) 0.82861(17) 0.0809(7) Uani 1 d U . .
C5 C 0.43489(11) 0.15169(13) 0.78872(15) 0.0696(6) Uani 1 d U . .
H5 H 0.4764 0.1753 0.8192 0.084 Uiso 1 calc R . .
C6 C 0.39976(10) 0.18174(11) 0.70402(14) 0.0553(5) Uani 1 d U . .
C7 C 0.43158(14) 0.2500 0.6582(2) 0.0554(7) Uani 1 d SU . .
H7A H 0.4205 0.2500 0.5857 0.067 Uiso 1 calc SR . .
H7B H 0.4875 0.2500 0.6662 0.067 Uiso 1 calc SR . .
C14 C 0.25011(13) 0.03359(12) 0.64045(18) 0.0759(6) Uani 1 d U . .
C15 C 0.27225(17) 0.02218(15) 0.5279(2) 0.1032(9) Uani 1 d U . .
H15A H 0.2732 0.0676 0.4935 0.155 Uiso 1 calc R . .
H15B H 0.2347 -0.0085 0.4960 0.155 Uiso 1 calc R . .
H15C H 0.3226 0.0004 0.5241 0.155 Uiso 1 calc R . .
C16 C 0.17135(13) 0.07006(17) 0.6471(2) 0.1195(11) Uani 1 d U . .
H16A H 0.1598 0.0808 0.7170 0.179 Uiso 1 calc R . .
H16B H 0.1322 0.0387 0.6201 0.179 Uiso 1 calc R . .
H16C H 0.1723 0.1137 0.6083 0.179 Uiso 1 calc R . .
C17 C 0.2420(2) -0.04098(16) 0.6873(3) 0.1335(12) Uani 1 d U . .
H17A H 0.2906 -0.0659 0.6822 0.200 Uiso 1 calc R . .
H17B H 0.2027 -0.0673 0.6514 0.200 Uiso 1 calc R . .
H17C H 0.2276 -0.0366 0.7577 0.200 Uiso 1 calc R . .
C18 C 0.44855(17) 0.05505(19) 0.9212(2) 0.1284(12) Uani 1 d U . .
H18A H 0.4487 0.0038 0.9146 0.193 Uiso 1 calc R . .
H18B H 0.4204 0.0684 0.9815 0.193 Uiso 1 calc R . .
H18C H 0.5010 0.0721 0.9262 0.193 Uiso 1 calc R . .
C1S C 0.5050(9) -0.0333(14) 0.5546(15) 0.235(7) Uani 0.50 d PDU D -1
C2S C 0.507(2) 0.0382(14) 0.5656(15) 0.240(9) Uani 0.50 d PDU D -1
H2S H 0.5127 0.0588 0.6297 0.288 Uiso 0.50 calc PR D -1
C3S C 0.4988(15) 0.0804(14) 0.4803(17) 0.256(8) Uani 0.50 d PDU D -1
H3S H 0.5076 0.1296 0.4831 0.307 Uiso 0.50 calc PR D -1
C4S C 0.4786(17) 0.0490(16) 0.3945(14) 0.273(9) Uani 0.50 d PDU D -1
H4S H 0.4639 0.0768 0.3389 0.327 Uiso 0.50 calc PR D -1
C5S C 0.4790(16) -0.0211(17) 0.3865(15) 0.250(9) Uani 0.50 d PDU D -1
H5S H 0.4711 -0.0414 0.3225 0.300 Uiso 0.50 calc PR D -1
C6S C 0.4900(16) -0.0642(15) 0.4646(18) 0.256(8) Uani 0.50 d PDU D -1
H6S H 0.4874 -0.1138 0.4576 0.308 Uiso 0.50 calc PR D -1
C7S C 0.5111(19) -0.0795(16) 0.6371(16) 0.416(15) Uani 0.50 d PDU D -1
H7S1 H 0.5070 -0.1281 0.6139 0.623 Uiso 0.50 calc PR D -1
H7S2 H 0.4702 -0.0697 0.6848 0.623 Uiso 0.50 calc PR D -1
H7S3 H 0.5604 -0.0727 0.6699 0.623 Uiso 0.50 calc PR D -1
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
_geom_angle_publ_flag
O1 P O1 116.36(9) 7_565 . ?
O1 P N1 121.82(5) 7_565 . ?
O1 P N1 121.82(5) . . ?
O1 P O2 92.07(5) 7_565 . ?
O1 P O2 92.07(5) . . ?
N1 P O2 85.14(9) . . ?
O1 P N3 89.32(6) 7_565 . ?
O1 P N3 89.32(6) . . ?
N1 P N3 92.22(11) . . ?
O2 P N3 177.36(10) . . ?
C1 O1 P 127.61(12) . . ?
C24 O2 P 112.31(15) . . ?
N2 C24 O3 121.1(2) . . ?
N2 C24 O2 120.2(2) . . ?
O3 C24 O2 118.7(2) . . ?
C24 N2 N1 104.41(19) . . ?
N2 N1 C28 109.5(2) . . ?
N2 N1 C28 109.5(2) . 7_565 ?
C28 N1 C28 50.5(4) . 7_565 ?
N2 N1 P 117.91(15) . . ?
C28 N1 P 125.9(2) . . ?
C28 N1 P 125.9(2) 7_565 . ?
C24 O3 C25 119.5(2) . 7_565 ?
C24 O3 C25 119.5(2) . . ?
C25 O3 C25 8.7(11) 7_565 . ?
O3 C25 C27 104.6(7) . . ?
O3 C25 C26 108.2(5) . . ?
C27 C25 C26 112.9(6) . . ?
O4 C28 O5 125.0(4) . . ?
O4 C28 N1 128.9(4) . . ?
O5 C28 N1 106.0(3) . . ?
C28 O5 C28 62.9(4) 7_565 . ?
C28 O5 C29 136.4(4) 7_565 . ?
C28 O5 C29 119.6(5) . . ?
C28 O5 C29 119.6(5) 7_565 7_565 ?
C28 O5 C29 136.4(4) . 7_565 ?
C29 O5 C29 25.4(11) . 7_565 ?
C30 C29 O5 107.3(7) . . ?
C30 C29 C31 113.3(12) . . ?
O5 C29 C31 104.2(5) . . ?
C34 N3 C34 82.4(4) 7_565 . ?
C34 N3 C32 104.1(3) 7_565 7_565 ?
C34 N3 C32 47.8(3) . 7_565 ?
C34 N3 C32 47.8(3) 7_565 . ?
C34 N3 C32 104.1(3) . . ?
C32 N3 C32 87.9(4) 7_565 . ?
C34 N3 P 127.8(2) 7_565 . ?
C34 N3 P 127.8(2) . . ?
C32 N3 P 128.0(2) 7_565 . ?
C32 N3 P 128.0(2) . . ?
N4 C32 N3 109.8(5) . . ?
C32 N4 C33 105.0(8) . . ?
N3 C34 C33 111.1(5) . . ?
C34 C33 N4 109.8(9) . . ?
C6 C1 C2 123.13(18) . . ?
C6 C1 O1 116.53(17) . . ?
C2 C1 O1 120.08(17) . . ?
C3 C2 C1 115.28(19) . . ?
C3 C2 C14 120.5(2) . . ?
C1 C2 C14 124.24(19) . . ?
C4 C3 C2 123.4(2) . . ?
C5 C4 C3 118.5(2) . . ?
C5 C4 C18 121.5(2) . . ?
C3 C4 C18 120.0(2) . . ?
C4 C5 C6 121.5(2) . . ?
C5 C6 C1 117.95(19) . . ?
C5 C6 C7 120.12(19) . . ?
C1 C6 C7 121.88(18) . . ?
C6 C7 C6 114.9(2) . 7_565 ?
C16 C14 C17 107.7(2) . . ?
C16 C14 C2 110.9(2) . . ?
C17 C14 C2 112.1(2) . . ?
C16 C14 C15 109.7(2) . . ?
C17 C14 C15 106.4(2) . . ?
C2 C14 C15 109.90(19) . . ?
C6S C1S C2S 121.8(12) . . ?
C6S C1S C7S 115.8(17) . . ?
C2S C1S C7S 122.1(16) . . ?
C1S C2S C3S 118.7(11) . . ?
C4S C3S C2S 117.8(13) . . ?
C5S C4S C3S 120.7(14) . . ?
C4S C5S C6S 123.2(15) . . ?
C5S C6S C1S 116.8(13) . . ?
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
P O1 1.5873(13) 7_565 ?
P O1 1.5873(13) . ?
P N1 1.674(2) . ?
P O2 1.7306(18) . ?
P N3 1.752(2) . ?
O1 C1 1.417(2) . ?
O2 C24 1.315(3) . ?
C24 N2 1.274(3) . ?
C24 O3 1.313(3) . ?
N2 N1 1.427(3) . ?
N1 C28 1.516(4) . ?
N1 C28 1.516(4) 7_565 ?
O3 C25 1.465(4) 7_565 ?
O3 C25 1.465(4) . ?
C25 C27 1.498(12) . ?
C25 C26 1.506(8) . ?
C28 O4 1.180(5) . ?
C28 O5 1.241(4) . ?
O5 C28 1.241(4) 7_565 ?
O5 C29 1.482(5) . ?
O5 C29 1.482(5) 7_565 ?
C29 C30 1.473(12) . ?
C29 C31 1.509(8) . ?
N3 C34 1.266(4) 7_565 ?
N3 C34 1.266(4) . ?
N3 C32 1.466(5) 7_565 ?
N3 C32 1.466(5) . ?
C32 N4 1.290(8) . ?
N4 C33 1.371(7) . ?
C34 C33 1.334(10) . ?
C1 C6 1.388(3) . ?
C1 C2 1.396(3) . ?
C2 C3 1.388(3) . ?
C2 C14 1.535(3) . ?
C3 C4 1.385(3) . ?
C4 C5 1.367(3) . ?
C4 C18 1.514(3) . ?
C5 C6 1.384(3) . ?
C6 C7 1.511(2) . ?
C7 C6 1.511(2) 7_565 ?
C14 C16 1.521(3) . ?
C14 C17 1.527(3) . ?
C14 C15 1.539(3) . ?
C1S C6S 1.339(12) . ?
C1S C2S 1.343(12) . ?
C1S C7S 1.39(3) . ?
C2S C3S 1.376(12) . ?
C3S C4S 1.315(12) . ?
C4S C5S 1.314(13) . ?
C5S C6S 1.316(12) . ?
