#------------------------------------------------------------------------------
#$Date: 2016-02-14 16:26:36 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176435 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/83/2238326.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2238326
loop_
_publ_author_name
'Schilling, Lars-Hendrik'
'Stock, Norbert'
_publ_section_title
;
 catena-Poly[[[tetraaquamagnesium]-trans-μ-[(piperazine-1,4-diium-1,4-diyl)bis(methylene)]diphosphonato]
 hemihydrate]
;
_journal_coeditor_code           CQ2003
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m452
_journal_page_last               m453
_journal_paper_doi               10.1107/S1600536813018722
_journal_volume                  69
_journal_year                    2013
_chemical_formula_iupac          '[Mg (C6 H14 N2 O6 P2) (H2 O1)4], 0.5H2 O1'
_chemical_formula_moiety         'C6 H22 Mg N2 O10 P2, H O0.5'
_chemical_formula_sum            'C6 H23 Mg N2 O10.5 P2'
_chemical_formula_weight         377.51
_chemical_name_systematic
'catena-Poly[[[tetraaquamagnesium]-trans-μ-[(piperazine-1,4-diium-1,4-diyl)bis(methylene)]diphosphonato] hemihydrate]'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.579(6)
_cell_angle_beta                 103.326(6)
_cell_angle_gamma                106.552(6)
_cell_formula_units_Z            1
_cell_length_a                   6.6296(5)
_cell_length_b                   6.8074(6)
_cell_length_c                   8.7962(7)
_cell_measurement_reflns_used    1270
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.77
_cell_measurement_theta_min      1.15
_cell_volume                     365.75(5)
_computing_cell_refinement       'X-AREA (Stoe & Cie, 2008)'
_computing_data_collection       'X-AREA (Stoe & Cie, 2008)'
_computing_data_reduction        'X-AREA (Stoe & Cie, 2008)'
_computing_molecular_graphics
;
XP in SHELXTL (Sheldrick, 2008) and DIAMOND Brandenburg (2011);
;
_computing_publication_material  'XCIF in SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Stoe IPSD-2'
_diffrn_measurement_method       'omega scan'
_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  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6973
_diffrn_reflns_theta_full        29.16
_diffrn_reflns_theta_max         29.16
_diffrn_reflns_theta_min         3.16
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.396
_exptl_absorpt_correction_T_max  0.9741
_exptl_absorpt_correction_T_min  0.8857
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(X-SHAPE and X-RED32; Stoe & Cie, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.714
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             199
_exptl_crystal_size_max          0.2053
_exptl_crystal_size_mid          0.1228
_exptl_crystal_size_min          0.0402
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.434
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     103
_refine_ls_number_reflns         1957
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0298
_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)+(0.0352P)²+0.2734P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0799
_reflns_number_gt                1727
_reflns_number_total             1957
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            cq2003.cif
_cod_data_source_block           I
_cod_original_formula_sum        'C6 H23 Mg N2 O10.50 P2'
_cod_database_code               2238326
_cod_database_fobs_code          2238326
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_symmetry_multiplicity
Mg Mg1 0.5000 0.5000 0.5000 0.01868(16) Uani d S 1 2
P P1 0.36611(6) 0.83891(6) 0.71790(4) 0.01741(10) Uani d . 1 1
O O1 0.47100(19) 0.67534(18) 0.69031(14) 0.0256(2) Uani d . 1 1
O O2 0.22643(18) 0.87610(17) 0.56605(13) 0.0228(2) Uani d . 1 1
O O3 0.52336(14) 1.04094(13) 0.81824(11) 0.0225(2) Uani d . 1 1
C C1 0.17809(14) 0.73201(13) 0.83666(11) 0.0218(3) Uani d R 1 1
H H1A 0.2264 0.6279 0.8904 0.026 Uiso d R 1 1
H H1B 0.0379 0.6240 0.8034 0.026 Uiso d R 1 1
N N1 0.1348(2) 0.89184(19) 0.94153(15) 0.0181(2) Uani d . 1 1
H H1N1 0.2589 0.9558 1.0077 0.022 Uiso d R 1 1
C C2 0.0614(3) 1.0529(2) 0.85892(19) 0.0235(3) Uani d . 1 1
H H2A -0.0754 0.9870 0.7791 0.028 Uiso calc R 1 1
H H2B 0.1690 1.1225 0.8065 0.028 Uiso calc R 1 1
C C3 -0.0313(3) 0.7900(2) 1.02369(19) 0.0218(3) Uani d . 1 1
H H3A 0.0147 0.6857 1.0786 0.026 Uiso calc R 1 1
H H3B -0.1695 0.7211 0.9461 0.026 Uiso calc R 1 1
O O4 0.30950(18) 0.64149(17) 0.34463(13) 0.0236(2) Uani d . 1 1
H H1O4 0.3778 0.7291 0.3008 0.028 Uiso d R 1 1
H H2O4 0.2647 0.7153 0.3980 0.028 Uiso d R 1 1
O O5 0.22487(19) 0.26098(18) 0.51161(16) 0.0309(3) Uani d . 1 1
H H1O5 0.2383 0.1488 0.5310 0.037 Uiso d R 1 1
H H2O5 0.0957 0.2540 0.4922 0.037 Uiso d R 1 1
O O6 0.5116(13) 0.5606(12) 1.0711(9) 0.0620(19) Uani d P 0.25 1
H H1O6 0.5284 0.5120 1.1538 0.093 Uiso d PR 0.25 1
H H2O6 0.5205 0.6822 1.0956 0.093 Uiso d PR 0.25 1
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'
Mg Mg 0.0486 0.0363 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
O1 Mg1 O1 2_666 . 180.00(6)
O1 Mg1 O5 2_666 . 90.35(5)
O1 Mg1 O5 . . 89.65(5)
O1 Mg1 O5 2_666 2_666 89.65(5)
O1 Mg1 O5 . 2_666 90.35(5)
O5 Mg1 O5 . 2_666 180.00(7)
O1 Mg1 O4 2_666 2_666 89.80(4)
O1 Mg1 O4 . 2_666 90.20(4)
O5 Mg1 O4 . 2_666 87.19(5)
O5 Mg1 O4 2_666 2_666 92.81(5)
O1 Mg1 O4 2_666 . 90.20(4)
O1 Mg1 O4 . . 89.80(4)
O5 Mg1 O4 . . 92.81(5)
O5 Mg1 O4 2_666 . 87.19(5)
O4 Mg1 O4 2_666 . 180.0
O1 P1 O2 . . 113.06(7)
O1 P1 O3 . . 114.25(6)
O2 P1 O3 . . 112.00(6)
O1 P1 C1 . . 105.10(6)
O2 P1 C1 . . 106.31(6)
O3 P1 C1 . . 105.20(5)
P1 O1 Mg1 . . 137.40(7)
N1 C1 P1 . . 114.69(7)
N1 C1 H1A . . 114.7
P1 C1 H1A . . 108.7
N1 C1 H1B . . 102.6
P1 C1 H1B . . 128.8
H1A C1 H1B . . 83.9
C3 N1 C2 . . 108.49(11)
C3 N1 C1 . . 110.46(10)
C2 N1 C1 . . 114.75(11)
C3 N1 H1N1 . . 111.5
C2 N1 H1N1 . . 106.5
C1 N1 H1N1 . . 105.1
N1 C2 C3 . 2_577 110.27(12)
N1 C2 H2A . . 109.6
C3 C2 H2A 2_577 . 109.6
N1 C2 H2B . . 109.6
C3 C2 H2B 2_577 . 109.6
H2A C2 H2B . . 108.1
N1 C3 C2 . 2_577 111.06(12)
N1 C3 H3A . . 109.4
C2 C3 H3A 2_577 . 109.4
N1 C3 H3B . . 109.4
C2 C3 H3B 2_577 . 109.4
H3A C3 H3B . . 108.0
Mg1 O4 H1O4 . . 115.4
Mg1 O4 H2O4 . . 108.1
H1O4 O4 H2O4 . . 99.6
Mg1 O5 H1O5 . . 119.2
Mg1 O5 H2O5 . . 130.9
H1O5 O5 H2O5 . . 109.7
O6 O6 H1O6 2_667 . 119.9
O6 O6 H2O6 2_667 . 133.7
H1O6 O6 H2O6 . . 106.3
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mg1 O1 2_666 2.0552(11)
Mg1 O1 . 2.0553(11)
Mg1 O5 . 2.0991(12)
Mg1 O5 2_666 2.0992(12)
Mg1 O4 2_666 2.1209(11)
Mg1 O4 . 2.1209(11)
P1 O1 . 1.5027(11)
P1 O2 . 1.5242(12)
P1 O3 . 1.5240(10)
P1 C1 . 1.8383
C1 N1 . 1.5022(15)
C1 H1A . 0.9700
C1 H1B . 0.9700
N1 C3 . 1.4925(18)
N1 C2 . 1.495(2)
N1 H1N1 . 0.8600
C2 C3 2_577 1.513(2)
C2 H2A . 0.9700
C2 H2B . 0.9700
C3 C2 2_577 1.513(2)
C3 H3A . 0.9700
C3 H3B . 0.9700
O4 H1O4 . 0.8199
O4 H2O4 . 0.8201
O5 H1O5 . 0.8200
O5 H2O5 . 0.8200
O6 O6 2_667 1.395(16)
O6 H1O6 . 0.8201
O6 H2O6 . 0.8200
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1N1 O3 2_677 0.86 1.84 2.6187(16) 150
O4 H1O4 O3 2_676 0.82 1.99 2.7956(15) 166
O4 H2O4 O2 . 0.82 1.88 2.6733(17) 164
O5 H1O5 O2 1_545 0.82 1.89 2.7032(17) 172
O5 H2O5 O2 2_566 0.82 1.99 2.7667(18) 158
C1 H1B O4 2_566 0.97 2.48 3.4279(15) 166
C2 H2B O3 . 0.97 2.55 3.187(2) 124
