#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/01/4000105.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_4000105
_journal_name_full               'Chemistry of Materials'
_journal_year                    2001
_chemical_formula_sum            'B Fe H5 N O9 P2'
_chemical_formula_weight         291.65
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 102.049(13)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3698(11)
_cell_length_b                   8.3092(15)
_cell_length_c                   9.6800(10)
_cell_measurement_reflns_used    ?
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      ?
_cell_measurement_theta_min      ?
_cell_volume                     737.04(18)
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           AgK\a
_diffrn_radiation_wavelength     0.56087
_diffrn_reflns_av_R_equivalents  0.1086
_diffrn_reflns_av_sigmaI/netI    0.1174
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11236
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    1.300
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_process_details   ?
_exptl_crystal_colour            pale-pink
_exptl_crystal_density_diffrn    2.628
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod-shaped
_exptl_crystal_F_000             580
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.864
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         2849
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      0.862
_refine_ls_R_factor_all          0.0891
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0207P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0596
_refine_ls_wR_factor_ref         0.0674
_reflns_number_gt                1761
_reflns_number_total             2849
_reflns_threshold_expression     >2sigma(I)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'H5 B Fe N O9 P2'
_cod_database_code               4000105
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
Fe1 Fe 0.78816(4) 0.15318(5) 0.57040(5) 0.00408(9) Uani 1 1 d . . .
B1 B 0.6667(3) 0.5627(4) 0.8096(4) 0.0065(6) Uani 1 1 d . . .
P1 P 0.92451(7) 0.06225(9) 0.29564(8) 0.00376(14) Uani 1 1 d . . .
P2 P 0.57801(7) 0.24272(9) 0.78467(8) 0.00407(14) Uani 1 1 d . . .
O1 O 0.9090(2) 0.1658(3) 0.4219(2) 0.0083(4) Uani 1 1 d . . .
O2 O 0.9229(2) 0.0059(2) 0.6917(2) 0.0081(4) Uani 1 1 d . . .
O3 O 0.8883(2) 0.3462(3) 0.6559(2) 0.0081(4) Uani 1 1 d . . .
O4 O 0.6547(2) 0.1286(2) 0.7022(2) 0.0091(4) Uani 1 1 d . . .
O5 O 0.5923(2) 0.4202(2) 0.7380(2) 0.0069(4) Uani 1 1 d . . .
O6 O 0.8145(2) -0.0820(2) 0.2830(2) 0.0076(4) Uani 1 1 d . . .
O7 O 0.4104(2) 0.2107(2) 0.7447(2) 0.0082(4) Uani 1 1 d . . .
O8 O 0.6292(2) 0.2764(3) 0.4425(2) 0.0099(4) Uani 1 1 d . . .
O9 O 0.6814(2) 0.5525(3) 0.9644(2) 0.0086(4) Uani 1 1 d . . .
H1 H 0.610(4) 0.578(4) 0.991(4) 0.013 Uiso 1 1 d . . .
N1 N 0.8167(3) 0.5967(4) 0.4388(4) 0.0211(7) Uiso 1 1 d D . .
H2 H 0.827(3) 0.520(3) 0.495(3) 0.025 Uiso 1 1 d D . .
H3 H 0.875(3) 0.666(3) 0.470(3) 0.025 Uiso 1 1 d D . .
H4 H 0.734(2) 0.625(4) 0.421(3) 0.025 Uiso 1 1 d D . .
H5 H 0.840(3) 0.562(4) 0.365(3) 0.025 Uiso 1 1 d D . .
