#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:53:07 +0100 (mar 22 de mar de 2016) $
#$Revision: 179133 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/95/4309540.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_4309540
loop_
_publ_author_name
'Ramasamy Pothiraja'
'Malaichamy Sathiyendiran'
'Ray J. Butcher'
'Ramaswamy Murugavel'
_publ_section_title
;
Non-Interpenetrating Transition Metal Diorganophosphate 2-Dimensional
Rectangular Grids from Their 1-Dimensional Wires: Structural
Transformations under Mild Conditions
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6314
_journal_page_last               6323
_journal_paper_doi               10.1021/ic050742z
_journal_volume                  44
_journal_year                    2005
_chemical_formula_sum            'C10 H14 N2 O8 P2'
_chemical_formula_weight         352.17
_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                 98.55(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   4.67400(10)
_cell_length_b                   18.036(8)
_cell_length_c                   8.161(2)
_cell_measurement_temperature    133(2)
_cell_volume                     680.3(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0377
_diffrn_reflns_av_sigmaI/netI    0.0176
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            6793
_diffrn_reflns_theta_full        24.67
_diffrn_reflns_theta_max         24.67
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    0.365
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.249
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         1157
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0283
_refine_ls_R_factor_gt           0.0258
_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)+(0.0306P)²+0.4738P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0656
_refine_ls_wR_factor_ref         0.0671
_reflns_number_gt                1079
_reflns_number_total             1157
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic050742zsi20050511_053247_5.cif
_cod_data_source_block           mur60(Compound7,Organic_phosphate)
_cod_original_cell_volume        680.4(4)
_cod_database_code               4309540
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
P1 P 0.36453(8) 0.68866(2) 0.96021(5) 0.01323(16) Uani 1 1 d . . .
O2 O 0.6080(3) 0.74770(7) 0.95851(18) 0.0280(3) Uani 1 1 d . . .
O3 O 0.4739(2) 0.61474(6) 1.02662(14) 0.0204(3) Uani 1 1 d . . .
O1 O 0.2286(3) 0.67458(7) 0.77564(15) 0.0240(3) Uani 1 1 d . . .
O4 O 0.1386(2) 0.72372(7) 1.05043(14) 0.0186(3) Uani 1 1 d . . .
N1 N 0.9112(3) 0.56659(8) 1.22226(17) 0.0153(3) Uani 1 1 d . . .
C1 C 1.0594(4) 0.61300(9) 1.3315(2) 0.0173(4) Uani 1 1 d . . .
C2 C 1.2927(4) 0.58840(9) 1.4407(2) 0.0164(3) Uani 1 1 d . . .
C3 C 1.3764(3) 0.51424(9) 1.43948(18) 0.0128(3) Uani 1 1 d . . .
C4 C 1.2195(4) 0.46742(9) 1.3221(2) 0.0181(4) Uani 1 1 d . . .
C5 C 0.9869(4) 0.49521(9) 1.2154(2) 0.0185(4) Uani 1 1 d . . .
H1B H 0.994(4) 0.6639(11) 1.329(2) 0.018(5) Uiso 1 1 d . . .
H4B H 1.265(4) 0.4150(12) 1.314(2) 0.022(5) Uiso 1 1 d . . .
H5B H 0.867(4) 0.4645(10) 1.138(2) 0.019(5) Uiso 1 1 d . . .
H2B H 1.386(4) 0.6218(12) 1.513(3) 0.026(5) Uiso 1 1 d . . .
H1A H 0.741(5) 0.5856(14) 1.145(3) 0.047(7) Uiso 1 1 d . . .
H1 H 0.220(5) 0.7096(14) 0.720(3) 0.038(7) Uiso 1 1 d . . .
H2 H 0.771(6) 0.7320(17) 0.990(3) 0.060(9) Uiso 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
P1 0.0107(2) 0.0139(2) 0.0145(2) 0.00057(15) 0.00008(16) 0.00064(15)
O2 0.0122(6) 0.0188(6) 0.0529(9) 0.0058(6) 0.0041(6) 0.0006(5)
O3 0.0163(6) 0.0183(6) 0.0245(6) 0.0023(5) -0.0045(5) 0.0004(5)
O1 0.0414(8) 0.0169(6) 0.0128(6) 0.0015(5) 0.0006(5) 0.0001(5)
O4 0.0136(6) 0.0243(6) 0.0176(6) -0.0047(5) 0.0011(5) -0.0002(5)
N1 0.0130(7) 0.0192(7) 0.0138(7) 0.0038(5) 0.0019(5) -0.0001(5)
C1 0.0200(9) 0.0160(8) 0.0161(8) 0.0009(6) 0.0028(6) 0.0024(7)
C2 0.0188(8) 0.0164(8) 0.0135(8) -0.0016(6) 0.0005(6) -0.0002(6)
C3 0.0113(8) 0.0173(8) 0.0105(8) 0.0016(6) 0.0041(6) -0.0010(6)
C4 0.0182(8) 0.0143(8) 0.0205(9) -0.0007(6) -0.0014(6) 0.0007(6)
C5 0.0175(8) 0.0181(8) 0.0184(8) -0.0004(7) -0.0019(7) -0.0027(7)
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
O3 P1 O4 114.88(7) . . ?
O3 P1 O2 113.58(7) . . ?
O4 P1 O2 106.37(7) . . ?
O3 P1 O1 105.74(7) . . ?
O4 P1 O1 108.86(7) . . ?
O2 P1 O1 107.11(8) . . ?
C1 N1 C5 121.05(15) . . ?
N1 C1 C2 120.79(16) . . ?
C1 C2 C3 120.08(15) . . ?
C2 C3 C4 117.69(14) . . ?
C2 C3 C3 121.00(18) . 3_868 ?
C4 C3 C3 121.31(18) . 3_868 ?
C5 C4 C3 119.70(15) . . ?
N1 C5 C4 120.68(16) . . ?
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
P1 O3 1.5000(13) . ?
P1 O4 1.5126(12) . ?
P1 O2 1.5602(13) . ?
P1 O1 1.5661(14) . ?
N1 C1 1.338(2) . ?
N1 C5 1.338(2) . ?
C1 C2 1.375(2) . ?
C2 C3 1.394(2) . ?
C3 C4 1.400(2) . ?
C3 C3 1.495(3) 3_868 ?
C4 C5 1.382(2) . ?
