#------------------------------------------------------------------------------
#$Date: 2016-03-21 01:21:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178377 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/02/4000299.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_4000299
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/cm030306f
_journal_year                    2003
_chemical_formula_moiety         'C4 H23 N4 O17 P4 Sc3'
_chemical_formula_sum            'C4 H29 N4 O21 P4 Sc3'
_chemical_formula_weight         728.07
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 96.877(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.603(2)
_cell_length_b                   15.476(3)
_cell_length_c                   16.504(4)
_cell_measurement_temperature    293(2)
_cell_measurement_wavelength     0.71073
_cell_volume                     2181.5(8)
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.922
_diffrn_measured_fraction_theta_max 0.922
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.04
_diffrn_reflns_av_unetI/netI     0.0419
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12138
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.31
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.217
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.012
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         4985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.085
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0764P)²+4.9158P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1383
_reflns_number_gt                4053
_reflns_number_total             4985
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4000299
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Sc1 Sc 0.63355(8) 0.79805(4) 0.16364(4) 0.01278(16) Uani 1 1 d . . .
Sc2 Sc 0.49585(8) 0.89323(4) 0.52210(4) 0.01201(16) Uani 1 1 d . . .
Sc3 Sc 1.02152(8) 0.76914(4) 0.29943(4) 0.01356(16) Uani 1 1 d . . .
P1 P 0.22760(11) 0.76200(6) 0.13355(6) 0.0147(2) Uani 1 1 d . . .
P2 P 0.26411(10) 0.71634(6) 0.47600(5) 0.0133(2) Uani 1 1 d . . .
P3 P 0.81649(11) 0.60698(6) 0.19758(5) 0.0140(2) Uani 1 1 d . . .
P4 P 0.66826(11) 0.79002(6) 0.37165(5) 0.0151(2) Uani 1 1 d . . .
O1 O 0.3708(2) 0.99391(13) 0.45826(12) 0.0052(4) Uani 1 1 d . . .
O2 O 0.6035(3) 0.86154(17) 0.42101(16) 0.0209(6) Uani 1 1 d . . .
O3 O 0.3147(3) 0.81082(17) 0.48960(16) 0.0194(5) Uani 1 1 d . . .
O4 O 0.5880(3) 0.79072(19) 0.28426(16) 0.0225(6) Uani 1 1 d . . .
O5 O 0.6605(3) 0.81028(17) 0.04101(16) 0.0194(6) Uani 1 1 d . . .
O6 O 0.4075(3) 0.92627(18) 0.63045(16) 0.0209(6) Uani 1 1 d . . .
O7 O 0.6546(3) 0.81416(18) 0.58558(17) 0.0243(6) Uani 1 1 d . . .
O8 O 0.8462(3) 0.79337(19) 0.37542(16) 0.0215(6) Uani 1 1 d . . .
O9 O 1.1036(3) 0.88146(15) 0.33821(15) 0.0136(5) Uani 1 1 d . . .
O10 O 0.8665(3) 0.81877(15) 0.20413(13) 0.0097(4) Uani 1 1 d . . .
O11 O 0.5942(3) 0.92567(15) 0.17168(14) 0.0134(5) Uani 1 1 d . . .
O12 O 0.9246(3) 0.64688(17) 0.26745(16) 0.0212(6) Uani 1 1 d . . .
O13 O 0.1684(3) 0.70545(17) 0.39177(16) 0.0196(6) Uani 1 1 d . . .
O14 O 0.4025(3) 0.7650(2) 0.12961(17) 0.0244(6) Uani 1 1 d . . .
O15 O 0.4091(3) 0.65773(18) 0.48163(17) 0.0224(6) Uani 1 1 d . . .
O16 O 0.6354(3) 0.69990(18) 0.40934(18) 0.0233(6) Uani 1 1 d . . .
H16 H 0.5453 0.6987 0.4209 0.08(3) Uiso 1 1 calc R . .
O17 O 0.6832(3) 0.66644(17) 0.16491(16) 0.0204(6) Uani 1 1 d . . .
O18 O 0.1930(3) 0.7606(2) 0.22181(17) 0.0254(6) Uani 1 1 d . . .
O19 O 0.1600(4) 0.84756(19) 0.0925(2) 0.0314(7) Uani 1 1 d . . .
H19 H 0.0755 0.8375 0.0656 0.046(17) Uiso 1 1 calc R . .
O20 O 0.7298(3) 0.52811(19) 0.23276(18) 0.0249(6) Uani 1 1 d . . .
H20 H 0.7945 0.4956 0.2573 0.06(2) Uiso 1 1 calc R . .
N1 N 1.3647(4) 0.9423(2) 0.2903(2) 0.0217(7) Uani 1 1 d . . .
H1A H 1.4241 0.9735 0.3273 0.06(2) Uiso 1 1 calc R . .
H1B H 1.4247 0.9053 0.2668 0.07(2) Uiso 1 1 calc R . .
H1C H 1.294 0.9131 0.3146 0.022(12) Uiso 1 1 calc R . .
N2 N 0.4073(5) 0.6187(3) 0.2922(3) 0.0373(10) Uani 1 1 d . . .
H3A H 0.3341 0.6492 0.3132 0.11(3) Uiso 1 1 calc R . .
H3B H 0.4674 0.654 0.2669 0.07(2) Uiso 1 1 calc R . .
H3C H 0.466 0.591 0.3321 0.17(5) Uiso 1 1 calc R . .
N3 N 0.9038(5) 0.5948(3) 0.4442(3) 0.0380(10) Uani 1 1 d . . .
H3A H 0.8074 0.6162 0.4424 0.046(17) Uiso 1 1 calc R . .
H3B H 0.9211 0.5785 0.3943 0.08(3) Uiso 1 1 calc R . .
H3C H 0.973 0.6352 0.4624 0.057(19) Uiso 1 1 calc R . .
N4 N 1.0050(5) 0.8790(2) 0.5096(2) 0.0288(8) Uani 1 1 d . . .
C1 C 0.4204(5) 0.9803(3) -0.0006(3) 0.0257(9) Uani 1 1 d . . .
H5A H 0.4046 0.9623 0.0541 0.027(12) Uiso 1 1 calc R . .
H5B H 0.3411 1.023 -0.0186 0.047(16) Uiso 1 1 calc R . .
C2 C 1.2841(5) 1.0002(3) 0.2278(3) 0.0264(9) Uani 1 1 d . . .
H6A H 1.2297 0.9664 0.1837 0.021(11) Uiso 1 1 calc R . .
H6B H 1.3598 1.0368 0.2054 0.048(16) Uiso 1 1 calc R . .
C3 C 1.1683(6) 1.0552(3) 0.2670(3) 0.0314(10) Uani 1 1 d . . .
H7A H 1.089 1.0184 0.2861 0.043(15) Uiso 1 1 calc R . .
H7B H 1.2221 1.0854 0.3136 0.062(19) Uiso 1 1 calc R . .
C4 C 0.0092(7) 1.0292(4) 0.4644(3) 0.0251(11) Uani 0.75 1 d P . .
C5 C 0.040(3) 1.0300(14) 0.5231(15) 0.043(5) Uani 0.25 1 d P . .
O21 O 0.5782(6) 0.4906(3) 0.3939(4) 0.0805(16) Uani 1 1 d . . .
