#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/14/4001483.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_4001483
loop_
_publ_author_name
'Serre, Christian'
'Groves, John A.'
'Lightfoot, Philip'
'Slawin, Alexandra M. Z.'
'Wright, Paul A.'
'Stock, Norbert'
'Bein, Thomas'
'Haouas, Mohamed'
'Taulelle, Francis'
'Férey, Gérard'
_publ_section_title
;
 Synthesis, Structure and Properties of Related
 MicroporousN,N‘-Piperazinebismethylenephosphonates of Aluminum and
 Titanium
;
_journal_issue                   6
_journal_name_full               'Chemistry of Materials'
_journal_page_first              1451
_journal_paper_doi               10.1021/cm052149l
_journal_volume                  18
_journal_year                    2006
_chemical_formula_moiety         'C6 H25 Al1 N2 O11 P2'
_chemical_formula_sum            'C6 H19.5 Al N2 O9.25 P2'
_chemical_formula_weight         356.66
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 90.54(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.859(9)
_cell_length_b                   6.915(3)
_cell_length_c                   11.256(6)
_cell_measurement_reflns_used    3885
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      64.42
_cell_measurement_theta_min      4.04
_cell_volume                     1467.8(12)
_computing_cell_refinement       TwinSolve
_computing_data_collection       CrystalClear
_computing_data_reduction        TwinSolve
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.956
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1881
_diffrn_reflns_av_sigmaI/netI    0.0886
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9557
_diffrn_reflns_theta_full        68.03
_diffrn_reflns_theta_max         68.03
_diffrn_reflns_theta_min         3.93
_exptl_absorpt_coefficient_mu    3.731
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.0321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ' '
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.614
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             746
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.032
_refine_diff_density_min         -0.722
_refine_diff_density_rms         0.211
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.208
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     93
_refine_ls_number_reflns         1396
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.208
_refine_ls_R_factor_all          0.1651
_refine_ls_R_factor_gt           0.1387
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1400P)²+31.7014P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3233
_refine_ls_wR_factor_ref         0.3393
_reflns_number_gt                1089
_reflns_number_total             1396
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cm052149lsi20050927_090031.cif
_cod_data_source_block           phil
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        1467.8(13)
_cod_original_sg_symbol_H-M      'C  2 (b)'
_cod_original_formula_sum        'C6 H19.50 Al N2 O9.25 P2'
_cod_database_code               4001483
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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
P1 P 0.33253(18) 0.0000 0.6917(3) 0.0232(9) Uani 1 2 d S
P2 P 0.32848(18) 0.0000 0.3099(3) 0.0249(10) Uani 1 2 d S
Al1 Al 0.2500 0.2500 0.5000 0.0232(10) Uani 1 2 d S
O1 O 0.2121(5) 0.0000 0.5051(9) 0.026(2) Uani 1 2 d S
H3 H 0.172(7) 0.0000 0.515(11) 0.01(3) Uiso 1 2 d S
O2 O 0.3198(3) 0.1836(10) 0.6204(5) 0.0263(16) Uani 1 1 d .
O3 O 0.3154(3) 0.1813(10) 0.3813(6) 0.0284(17) Uani 1 1 d .
O4 O 0.4049(5) 0.0000 0.7489(8) 0.030(2) Uani 1 2 d S
O5 O 0.2921(5) 0.0000 0.1913(9) 0.032(2) Uani 1 2 d S
N1 N 0.4754(6) 0.0000 0.3761(10) 0.028(3) Uiso 1 2 d S
H1 H 0.5193 0.0000 0.3432 0.034 Uiso 1 2 calc SR
N2 N 0.2529(8) 0.154(2) 0.8845(13) 0.024(3) Uiso 0.50 1 d P
C1 C 0.4713(5) 0.1772(16) 0.4524(9) 0.031(2) Uiso 1 1 d .
H1A H 0.4252 0.1827 0.4897 0.038 Uiso 1 1 calc R
H1B H 0.4763 0.2913 0.4030 0.038 Uiso 1 1 calc R
C2 C 0.4241(7) 0.0000 0.2770(13) 0.029(3) Uiso 1 2 d S
H2A H 0.4337 -0.1128 0.2285 0.035 Uiso 0.50 1 calc PR
H2B H 0.4337 0.1128 0.2285 0.035 Uiso 0.50 1 calc PR
C3 C 0.2642(8) 0.0000 0.8053(14) 0.036(4) Uiso 1 2 d S
H3A H 0.2194 -0.0231 0.7647 0.043 Uiso 0.25 1 d PR
H3B H 0.2732 -0.1129 0.8543 0.043 Uiso 0.25 1 d PR
H3C H 0.2733 0.1127 0.8544 0.043 Uiso 0.25 1 d PR
H3D H 0.2195 0.0237 0.7645 0.043 Uiso 0.25 1 d PR
C4 C 0.3183(10) 0.213(3) 0.9512(18) 0.028(4) Uiso 0.50 1 d P
H4A H 0.3348 0.1063 1.0000 0.034 Uiso 0.50 1 d PR
H4B H 0.3554 0.2451 0.8955 0.034 Uiso 0.50 1 d PR
C5 C 0.1943(10) 0.123(3) 0.9695(17) 0.030(4) Uiso 0.50 1 d P
H5A H 0.1516 0.0903 0.9250 0.035 Uiso 0.50 1 d PR
H5B H 0.2064 0.0000 1.0188 0.035 Uiso 1 2 d SR
C4A C 0.1795 0.2855 1.0467 0.029 Uiso 0.00 1 d P
C5A C 0.3056 0.3841 1.0294 0.033 Uiso 0.00 1 d P
O100 O 0.4098(7) 0.5000 0.6842(11) 0.052(3) Uiso 1 2 d S
O101 O 0.5217(13) 0.5000 0.856(2) 0.060 Uiso 0.58(3) 2 d SP
O102 O 0.4591(14) 0.152(4) 0.965(2) 0.060 Uiso 0.345(18) 1 d P
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 '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
O4 P1 O2 111.4(3) . 6
O4 P1 O2 111.4(3) . .
O2 P1 O2 113.3(5) 6 .
O4 P1 C3 110.1(7) . .
O2 P1 C3 105.1(4) 6 .
O2 P1 C3 105.1(4) . .
O5 P2 O3 113.5(3) . .
O5 P2 O3 113.5(3) . 6
O3 P2 O3 112.2(5) . 6
O5 P2 C2 105.2(6) . .
O3 P2 C2 105.8(4) . .
O3 P2 C2 105.8(4) 6 .
O1 Al1 O1 180.000(1) 7_556 .
O1 Al1 O3 92.4(3) 7_556 7_556
O1 Al1 O3 87.6(3) . 7_556
O1 Al1 O3 87.6(3) 7_556 .
O1 Al1 O3 92.4(3) . .
O3 Al1 O3 180.000(1) 7_556 .
O1 Al1 O2 89.0(4) 7_556 .
O1 Al1 O2 91.0(4) . .
O3 Al1 O2 90.5(3) 7_556 .
O3 Al1 O2 89.5(3) . .
O1 Al1 O2 91.0(4) 7_556 7_556
O1 Al1 O2 89.0(4) . 7_556
O3 Al1 O2 89.5(3) 7_556 7_556
O3 Al1 O2 90.5(3) . 7_556
O2 Al1 O2 180.000(1) . 7_556
Al1 O1 Al1 134.9(6) . 4_546
Al1 O1 H3 112.5(4) . .
Al1 O1 H3 112.5(4) 4_546 .
P1 O2 Al1 132.1(4) . .
P2 O3 Al1 134.1(4) . .
C2 N1 C1 113.4(7) . .
C2 N1 C1 113.4(7) . 6
C1 N1 C1 109.7(11) . 6
C2 N1 H1 106.6 . .
C1 N1 H1 106.6 . .
C1 N1 H1 106.6 6 .
C5 N2 C4 109.4(15) . .
C5 N2 C5A 1.8(8) . 7_557
C4 N2 C5A 109.4(12) . 7_557
C5 N2 C4A 109.5(12) . 7_557
C4 N2 C4A 0.2(9) . 7_557
C5A N2 C4A 109.5(9) 7_557 7_557
C5 N2 H3C 142.4 . .
C4 N2 H3C 83.3 . .
C5A N2 H3C 140.7 7_557 .
C4A N2 H3C 83.2 7_557 .
N1 C1 C1 111.3(7) . 2_656
N1 C1 H1A 109.4 . .
C1 C1 H1A 109.4 2_656 .
N1 C1 H1B 109.4 . .
C1 C1 H1B 109.4 2_656 .
H1A C1 H1B 108.0 . .
N1 C2 P2 119.0(10) . .
N1 C2 H2A 107.6 . .
P2 C2 H2A 107.6 . .
N1 C2 H2B 107.6 . .
P2 C2 H2B 107.6 . .
H2A C2 H2B 107.0 . .
N2 C3 P1 123.8(9) 6 .
N2 C3 H3A 92.2 6 .
P1 C3 H3A 106.8 . .
N2 C3 H3B 19.4 6 .
P1 C3 H3B 106.1 . .
H3A C3 H3B 106.4 . .
N2 C3 H3C 105.9 6 .
P1 C3 H3C 106.1 . .
H3A C3 H3C 123.3 . .
H3B C3 H3C 107.0 . .
N2 C3 H3D 107.0 6 .
P1 C3 H3D 106.6 . .
H3A C3 H3D 19.2 . .
H3B C3 H3D 123.5 . .
H3C C3 H3D 106.4 . .
N2 C4 C5A 112.1(14) . .
N2 C4 H3C 22.3 . .
C5A C4 H3C 133.1 . .
N2 C4 H4A 109.6 . .
C5A C4 H4A 108.8 . .
H3C C4 H4A 103.2 . .
N2 C4 H4B 109.5 . .
C5A C4 H4B 108.8 . .
H3C C4 H4B 92.4 . .
H4A C4 H4B 108.0 . .
C4A C5 N2 114.8(15) . .
C4A C5 H5A 109.0 . .
N2 C5 H5A 108.8 . .
C4A C5 H5B 110.9 . .
N2 C5 H5B 107.6 . .
H5A C5 H5B 105.4 . .
C4 C4A C5 106(10) 7_557 .
C4 C4A C5A 106(10) 7_557 7_557
C5 C4A C5A 1.5(8) . 7_557
C4 C4A N2 5(10) 7_557 7_557
C5 C4A N2 110.4(10) . 7_557
C5A C4A N2 110.1(6) 7_557 7_557
C5 C5A C4A 52(10) 7_557 7_557
C5 C5A C4 52(10) 7_557 .
C4A C5A C4 1.8(7) 7_557 .
C5 C5A N2 72(10) 7_557 7_557
C4A C5A N2 112.3(6) 7_557 7_557
C4 C5A N2 111.4(10) . 7_557
C5 C5A C5A 165(10) 7_557 6_565
C4A C5A C5A 142.365(19) 7_557 6_565
C4 C5A C5A 142.3(8) . 6_565
N2 C5A C5A 100.2(6) 7_557 6_565
C5 C5A C5 164(10) 7_557 4_557
C4A C5A C5 142.8(7) 7_557 4_557
C4 C5A C5 142.7(11) . 4_557
N2 C5A C5 100.0(9) 7_557 4_557
C5A C5A C5 0.5(7) 6_565 4_557
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
P1 O4 1.504(11) .
P1 O2 1.520(7) 6
P1 O2 1.520(7) .
P1 C3 1.824(16) .
P2 O5 1.495(11) .
P2 O3 1.511(7) .
P2 O3 1.511(7) 6
P2 C2 1.844(15) .
Al1 O1 1.872(4) 7_556
Al1 O1 1.872(4) .
Al1 O3 1.888(6) 7_556
Al1 O3 1.888(6) .
Al1 O2 1.935(6) .
Al1 O2 1.935(6) 7_556
O1 Al1 1.872(4) 4_546
O1 H3 0.77(13) .
N1 C2 1.471(18) .
N1 C1 1.499(12) .
N1 C1 1.499(12) 6
N1 H1 0.9100 .
N2 C5 1.49(2) .
N2 C4 1.49(2) .
N2 C5A 1.499(15) 7_557
N2 C4A 1.541(15) 7_557
N2 H3C 0.5888 .
C1 C1 1.517(19) 2_656
C1 H1A 0.9700 .
C1 H1B 0.9700 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 N2 1.408(19) 6
C3 H3A 0.9700 .
C3 H3B 0.9700 .
C3 H3C 0.9700 .
C3 H3D 0.9700 .
C4 C5A 1.49(2) .
C4 H3C 1.5408 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C4A 1.45(2) .
C5 H5A 0.9700 .
C5 H5B 1.0380 .
C4A C4 0.048(19) 7_557
C4A C5A 1.4808(5) 7_557
C4A N2 1.541(15) 7_557
C5A C5 0.05(2) 7_557
C5A C4A 1.4808(5) 7_557
C5A N2 1.499(15) 7_557
C5A C5A 1.6024(7) 6_565
C5A C5 1.65(2) 4_557
O102 O102 1.73(5) 2_657
