#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:24:39 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179326 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/23/4322314.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_4322314
loop_
_publ_author_name
'Li-Min Zheng'
'Hui-Hua Song'
'Chia-Heir Lin'
'Sue-Lein Wang'
'Zheng Hu'
'Zhi Yu'
Xin
_publ_section_title
;
 [NH3(CH2)4NH3]Fe2[CH3C(OH)(PO3)(PO3H)]2.2H2O: A Novel Iron(II)
 Diphosphonate with a Supramolecular Open Network Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4618
_journal_page_last               4619
_journal_paper_doi               10.1021/ic990482j
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C8 H28 Fe2 N2 O16 P4'
_chemical_formula_weight         643.90
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 99.2790(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.5362(2)
_cell_length_b                   12.8676(5)
_cell_length_c                   15.4337(5)
_cell_measurement_reflns_used    4249
_cell_measurement_temperature    295
_cell_measurement_theta_max      25
_cell_measurement_theta_min      2.5
_cell_volume                     1085.07(7)
_computing_cell_refinement       'SMART (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SMART (Siemens, 1995)'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'Siemens SHELXTL'
_computing_structure_solution    'SHELXTL-PLUS (Siemens, 1994)'
_diffrn_ambient_temperature      295
_diffrn_measurement_device       'Siemens smart-CCD diffractometer'
_diffrn_measurement_method       'ω scans'
_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  0.0281
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6263
_diffrn_reflns_theta_max         27.97
_diffrn_reflns_theta_min         2.07
_exptl_absorpt_coefficient_mu    1.712
_exptl_absorpt_correction_T_max  0.9660
_exptl_absorpt_correction_T_min  0.8392
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            Transparent
_exptl_crystal_density_diffrn    1.971
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Acicular
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       0.0068(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.046
_refine_ls_goodness_of_fit_obs   1.102
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     146
_refine_ls_number_reflns         2364
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.0341
_refine_ls_R_factor_obs          0.0254
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0393P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0697
_refine_ls_wR_factor_obs         0.0668
_reflns_number_observed          1981
_reflns_number_total             2364
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990482j.cif
_cod_data_source_block           fe(ot09m)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+0.0000P] 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^)+(0.0393P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4322314
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Fe1 Fe 0.38814(5) 0.03357(2) 0.09076(2) 0.01418(11) Uani 1 d . .
P1 P 0.90020(10) 0.12016(4) 0.17583(3) 0.01496(14) Uani 1 d . .
P2 P 0.89329(10) -0.10132(4) 0.11290(3) 0.01293(13) Uani 1 d . .
O1 O 0.6767(3) 0.14325(11) 0.10803(9) 0.0184(3) Uani 1 d . .
O2 O 0.1459(3) 0.13425(11) 0.14760(10) 0.0220(3) Uani 1 d . .
O3 O 0.8762(3) 0.18421(12) 0.25888(10) 0.0255(4) Uani 1 d . .
O4 O 0.6844(3) -0.06727(11) 0.04185(9) 0.0163(3) Uani 1 d . .
O5 O 0.1494(3) -0.08967(11) 0.09234(10) 0.0201(3) Uani 1 d . .
O6 O 0.8431(3) -0.21440(11) 0.13702(10) 0.0218(3) Uani 1 d . .
O7 O 0.6084(3) -0.02148(11) 0.21864(10) 0.0193(3) Uani 1 d . .
O1W O 0.5522(3) -0.19418(14) 0.30063(15) 0.0456(5) Uani 1 d . .
N1 N 0.6111(3) 0.26783(13) -0.04178(13) 0.0237(4) Uani 1 d . .
C1 C 0.6652(5) 0.3814(2) -0.0399(2) 0.0294(6) Uani 1 d . .
C2 C 0.4749(5) 0.4415(2) -0.0011(2) 0.0279(5) Uani 1 d . .
C3 C 1.0357(4) -0.0445(2) 0.29027(14) 0.0236(5) Uani 1 d . .
C4 C 0.8631(4) -0.01636(15) 0.20639(13) 0.0142(4) Uani 1 d . .
H1 H 0.7396 0.2327 -0.0749 0.080 Uiso 1 d . .
H2 H 0.6201 0.2432 0.0088 0.080 Uiso 1 d . .
H3 H 0.4775 0.2571 -0.0693 0.080 Uiso 1 d . .
H4 H 0.8407 0.3963 -0.0058 0.080 Uiso 1 d . .
H5 H 0.6694 0.4068 -0.1004 0.080 Uiso 1 d . .
H6 H 0.4704 0.4229 0.0539 0.080 Uiso 1 d . .
H7 H 0.3206 0.4316 -0.0380 0.080 Uiso 1 d . .
H8 H 1.1864 -0.0346 0.2833 0.080 Uiso 1 d . .
H9 H 0.9958 -0.0043 0.3400 0.080 Uiso 1 d . .
H10 H 1.0230 -0.1093 0.3053 0.080 Uiso 1 d . .
H11 H 1.0094 0.2221 0.3007 0.080 Uiso 1 d . .
H12 H 0.5952 -0.0810 0.2421 0.080 Uiso 1 d . .
H1WA H 0.4525 -0.2321 0.2709 0.080 Uiso 1 d . .
H1WB H 0.6680 -0.2434 0.3089 0.080 Uiso 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'
Fe Fe 0.3463 0.8444 '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
O5 Fe1 O4 98.63(6) . 3_655 ?
O5 Fe1 O1 168.93(6) . . ?
O4 Fe1 O1 90.40(6) 3_655 . ?
O5 Fe1 O2 90.88(6) . . ?
O4 Fe1 O2 104.07(6) 3_655 . ?
O1 Fe1 O2 93.13(6) . . ?
O5 Fe1 O7 90.31(6) . . ?
O4 Fe1 O7 157.17(6) 3_655 . ?
O1 Fe1 O7 78.99(5) . . ?
O2 Fe1 O7 96.70(6) . . ?
O5 Fe1 O4 93.55(5) . . ?
O4 Fe1 O4 80.17(5) 3_655 . ?
O1 Fe1 O4 81.64(5) . . ?
O2 Fe1 O4 173.35(5) . . ?
O7 Fe1 O4 78.34(5) . . ?
O2 P1 O1 116.87(9) 1_655 . ?
O2 P1 O3 112.21(9) 1_655 . ?
O1 P1 O3 107.33(9) . . ?
O2 P1 C4 109.45(9) 1_655 . ?
O1 P1 C4 104.58(8) . . ?
O3 P1 C4 105.56(9) . . ?
O5 P2 O4 116.72(9) 1_655 . ?
O5 P2 O6 110.93(9) 1_655 . ?
O4 P2 O6 107.48(8) . . ?
O5 P2 C4 108.26(9) 1_655 . ?
O4 P2 C4 103.83(8) . . ?
O6 P2 C4 109.25(9) . . ?
P1 O1 Fe1 118.16(8) . . ?
P1 O2 Fe1 134.25(9) 1_455 . ?
P2 O4 Fe1 140.93(9) . 3_655 ?
P2 O4 Fe1 114.99(8) . . ?
Fe1 O4 Fe1 99.83(5) 3_655 . ?
P2 O5 Fe1 134.65(9) 1_455 . ?
C4 O7 Fe1 105.68(11) . . ?
N1 C1 C2 111.0(2) . . ?
C1 C2 C2 112.2(3) . 3_665 ?
O7 C4 C3 111.6(2) . . ?
O7 C4 P1 103.15(12) . . ?
C3 C4 P1 111.33(14) . . ?
O7 C4 P2 106.74(13) . . ?
C3 C4 P2 113.67(14) . . ?
P1 C4 P2 109.79(10) . . ?
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
Fe1 O5 2.0671(15) . ?
Fe1 O4 2.0672(14) 3_655 ?
Fe1 O1 2.1159(14) . ?
Fe1 O2 2.1507(15) . ?
Fe1 O7 2.2602(15) . ?
Fe1 O4 2.3114(14) . ?
P1 O2 1.505(2) 1_655 ?
P1 O1 1.5157(15) . ?
P1 O3 1.547(2) . ?
P1 C4 1.839(2) . ?
P2 O5 1.509(2) 1_655 ?
P2 O4 1.5240(14) . ?
P2 O6 1.5383(14) . ?
P2 C4 1.839(2) . ?
O2 P1 1.505(2) 1_455 ?
O4 Fe1 2.0672(14) 3_655 ?
O5 P2 1.509(2) 1_455 ?
O7 C4 1.454(2) . ?
N1 C1 1.491(3) . ?
C1 C2 1.507(3) . ?
C2 C2 1.531(4) 3_665 ?
C3 C4 1.524(3) . ?
