#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/09/2230979.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_2230979
loop_
_publ_author_name
'Assani, Abderrazzak'
'Saadi, Mohamed'
'Zriouil, Mohammed'
'El Ammari, Lahcen'
_publ_contact_author_address
;
Laboratoire de Chimie du Solide Appliquée,
Faculté des Sciences, Université Mohammed V-Agdal
Avenue Ibn Battouta, B.P. 1014, Rabat, Maroc
;
_publ_contact_author_email       abder_assani@yahoo.fr
_publ_contact_author_fax         '212 537 77 54 40'
_publ_contact_author_name        'Abderrazzak  Assani'
_publ_contact_author_phone       '212 537 77 54 40'
_publ_section_title
;
 Heptamagnesium bis(phosphate) tetrakis(hydrogen phosphate) with strong
 hydrogen bonds: Mg₇(PO₄)₂(HPO₄)₄
;
_journal_coeditor_code           BT5638
_journal_date_accepted           2011-09-06
_journal_date_recd_electronic    2011-09-05
_journal_issue                   10
_journal_name_full               'Acta Crystallographica, Section E'
_journal_page_first              i52
_journal_page_last               i52
_journal_paper_category          QI
_journal_paper_doi               10.1107/S1600536811036361
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          'Mg7 (P O4)2 (H P O4)4'
_chemical_formula_structural     'Mg7 (P O4)2 (P O3 OH)4'
_chemical_formula_sum            'H4 Mg7 O24 P6'
_chemical_formula_weight         744.02
_chemical_name_common            'magnesium hydrogen phosphate'
_chemical_name_systematic
;
Heptamagnesium bis(phosphate) tetrakis(hydrogen phosphate)
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                104.442(3)
_cell_angle_beta                 108.505(5)
_cell_angle_gamma                101.189(8)
_cell_formula_units_Z            1
_cell_length_a                   6.4204(5)
_cell_length_b                   7.8489(4)
_cell_length_c                   9.4315(5)
_cell_measurement_reflns_used    1923
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.42
_cell_volume                     416.70(5)
_computing_cell_refinement       'APEX2 (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics
'ORTEP-3 for Windows (Farrugia,1997) and DIAMOND (Brandenburg, 2006)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker X8 APEX Diffractometer'
_diffrn_measurement_method       'φ and 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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0272
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            9421
_diffrn_reflns_theta_full        27.56
_diffrn_reflns_theta_max         27.56
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    1.055
_exptl_absorpt_correction_T_max  0.929
_exptl_absorpt_correction_T_min  0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.965
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepipedic
_exptl_crystal_F_000             370
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.416
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         1923
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0304
_refine_ls_R_factor_gt           0.0259
_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)+(0.0325P)²+0.6237P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0691
_refine_ls_wR_factor_ref         0.0718
_reflns_number_gt                1715
_reflns_number_total             1923
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            bt5638.cif
_cod_data_source_block           I
_cod_original_cell_volume        416.70(4)
_cod_database_code               2230979
_cod_database_fobs_code          2230979
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 -0.38348(12) 0.54390(10) -0.10950(8) 0.00639(17) Uani d . 1 1
Mg Mg2 0.0000 0.0000 0.0000 0.0094(2) Uani d S 1 2
Mg Mg3 -0.05324(13) 0.28758(10) -0.51536(9) 0.00821(17) Uani d . 1 1
Mg Mg4 -0.27778(13) 0.19081(11) -0.28530(9) 0.00902(17) Uani d . 1 1
P P1 0.22691(9) 0.14512(8) -0.22413(6) 0.00561(13) Uani d . 1 1
P P2 0.08899(9) 0.58025(7) -0.17255(6) 0.00465(13) Uani d . 1 1
P P3 -0.59090(9) 0.23141(8) -0.62865(7) 0.00658(14) Uani d . 1 1
O O1 0.0189(3) 0.1762(2) -0.33779(18) 0.0081(3) Uani d . 1 1
O O2 0.2208(3) 0.1877(2) -0.05694(18) 0.0074(3) Uani d . 1 1
O O3 0.4517(3) 0.2446(2) -0.22968(18) 0.0077(3) Uani d . 1 1
O O4 0.2013(3) -0.0667(2) -0.27972(18) 0.0091(3) Uani d . 1 1
H H4 0.1828 -0.1148 -0.2104 0.011 Uiso d R 1 1
O O5 0.3069(3) 0.5385(2) -0.08555(18) 0.0068(3) Uani d . 1 1
O O6 0.0589(3) 0.5452(2) -0.34643(18) 0.0073(3) Uani d . 1 1
O O7 0.1098(3) 0.7857(2) -0.09645(19) 0.0094(3) Uani d . 1 1
O O8 -0.1240(3) 0.4602(2) -0.16487(18) 0.0070(3) Uani d . 1 1
O O9 -0.3803(3) 0.2112(2) -0.50853(19) 0.0104(3) Uani d . 1 1
O O10 -0.5267(3) 0.3827(2) -0.69363(19) 0.0106(3) Uani d . 1 1
O O11 -0.7360(3) 0.0488(2) -0.76029(19) 0.0097(3) Uani d . 1 1
O O12 -0.7344(3) 0.2950(2) -0.52719(19) 0.0111(3) Uani d . 1 1
H H12 -0.6495 0.3935 -0.4485 0.013 Uiso d R 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
O O 0.0106 0.0060 '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'
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
O10 Mg1 O5 2_464 2_565 177.45(7)
O10 Mg1 O5 2_464 1_455 93.60(7)
O5 Mg1 O5 2_565 1_455 84.54(7)
O10 Mg1 O8 2_464 . 89.62(7)
O5 Mg1 O8 2_565 . 91.62(7)
O5 Mg1 O8 1_455 . 161.77(7)
O10 Mg1 O2 2_464 2_565 97.16(7)
O5 Mg1 O2 2_565 2_565 84.67(7)
O5 Mg1 O2 1_455 2_565 92.32(7)
O8 Mg1 O2 . 2_565 105.09(7)
O10 Mg1 O3 2_464 1_455 96.93(7)
O5 Mg1 O3 2_565 1_455 81.15(6)
O5 Mg1 O3 1_455 1_455 83.53(6)
O8 Mg1 O3 . 1_455 78.27(6)
O2 Mg1 O3 2_565 1_455 165.53(7)
O7 Mg2 O7 1_545 2_565 180.00(7)
O7 Mg2 O2 1_545 . 91.18(6)
O7 Mg2 O2 2_565 . 88.82(6)
O7 Mg2 O2 1_545 2 88.82(6)
O7 Mg2 O2 2_565 2 91.18(6)
O2 Mg2 O2 . 2 180.00(7)
O7 Mg2 O11 1_545 2_454 90.17(6)
O7 Mg2 O11 2_565 2_454 89.83(6)
O2 Mg2 O11 . 2_454 85.85(6)
O2 Mg2 O11 2 2_454 94.15(6)
O7 Mg2 O11 1_545 1_656 89.83(6)
O7 Mg2 O11 2_565 1_656 90.17(6)
O2 Mg2 O11 . 1_656 94.15(6)
O2 Mg2 O11 2 1_656 85.85(6)
O11 Mg2 O11 2_454 1_656 180.00(8)
O4 Mg3 O1 2_554 . 104.92(7)
O4 Mg3 O6 2_554 . 165.27(8)
O1 Mg3 O6 . . 89.19(7)
O4 Mg3 O6 2_554 2_564 87.80(7)
O1 Mg3 O6 . 2_564 165.83(8)
O6 Mg3 O6 . 2_564 78.70(7)
O4 Mg3 O12 2_554 1_655 89.06(7)
O1 Mg3 O12 . 1_655 90.91(7)
O6 Mg3 O12 . 1_655 95.01(7)
O6 Mg3 O12 2_564 1_655 82.93(7)
O4 Mg3 O9 2_554 . 82.41(7)
O1 Mg3 O9 . . 80.21(7)
O6 Mg3 O9 . . 96.14(7)
O6 Mg3 O9 2_564 . 108.15(7)
O12 Mg3 O9 1_655 . 165.63(8)
O8 Mg4 O11 . 2_454 135.86(7)
O8 Mg4 O9 . . 97.00(7)
O11 Mg4 O9 2_454 . 124.27(7)
O8 Mg4 O3 . 1_455 83.43(7)
O11 Mg4 O3 2_454 1_455 102.94(7)
O9 Mg4 O3 . 1_455 98.66(7)
O8 Mg4 O1 . . 88.96(7)
O11 Mg4 O1 2_454 . 84.69(7)
O9 Mg4 O1 . . 79.14(7)
O3 Mg4 O1 1_455 . 171.78(7)
O3 P1 O1 . . 111.79(9)
O3 P1 O2 . . 114.92(9)
O1 P1 O2 . . 110.31(9)
O3 P1 O4 . . 106.96(9)
O1 P1 O4 . . 107.87(9)
O2 P1 O4 . . 104.43(9)
O5 P2 O6 . . 109.03(9)
O5 P2 O8 . . 111.40(9)
O6 P2 O8 . . 109.62(9)
O5 P2 O7 . . 109.95(9)
O6 P2 O7 . . 108.49(9)
O8 P2 O7 . . 108.30(9)
O10 P3 O11 . . 112.06(9)
O10 P3 O9 . . 112.08(9)
O11 P3 O9 . . 111.85(9)
O10 P3 O12 . . 107.28(9)
O11 P3 O12 . . 109.21(9)
O9 P3 O12 . . 103.90(9)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Mg1 O10 2_464 2.0235(17)
Mg1 O5 2_565 2.0462(17)
Mg1 O5 1_455 2.0643(17)
Mg1 O8 . 2.0698(17)
Mg1 O2 2_565 2.1093(17)
Mg1 O3 1_455 2.2065(17)
Mg2 O7 1_545 2.0630(16)
Mg2 O7 2_565 2.0630(16)
Mg2 O2 . 2.1296(15)
Mg2 O2 2 2.1296(15)
Mg2 O11 2_454 2.2395(16)
Mg2 O11 1_656 2.2395(16)
Mg3 O4 2_554 2.0415(17)
Mg3 O1 . 2.0443(17)
Mg3 O6 . 2.0606(17)
Mg3 O6 2_564 2.0649(17)
Mg3 O12 1_655 2.0759(17)
Mg3 O9 . 2.0954(17)
Mg4 O8 . 2.0041(17)
Mg4 O11 2_454 2.0426(18)
Mg4 O9 . 2.0544(17)
Mg4 O3 1_455 2.0549(17)
Mg4 O1 . 2.1312(17)
P1 O3 . 1.5252(16)
P1 O1 . 1.5297(16)
P1 O2 . 1.5431(16)
P1 O4 . 1.5718(16)
P2 O5 . 1.5237(16)
P2 O6 . 1.5350(16)
P2 O8 . 1.5362(16)
P2 O7 . 1.5533(16)
P3 O10 . 1.5131(16)
P3 O11 . 1.5245(17)
P3 O9 . 1.5287(16)
P3 O12 . 1.5853(17)
O2 Mg1 2_565 2.1093(17)
O3 Mg4 1_655 2.0549(17)
O3 Mg1 1_655 2.2065(17)
O4 Mg3 2_554 2.0415(17)
O4 H4 . 0.8601
O5 Mg1 2_565 2.0462(17)
O5 Mg1 1_655 2.0643(17)
O6 Mg3 2_564 2.0649(17)
O7 Mg2 1_565 2.0630(16)
O10 Mg1 2_464 2.0235(17)
O11 Mg4 2_454 2.0426(18)
O11 Mg2 1_454 2.2395(16)
O12 Mg3 1_455 2.0759(17)
O12 H12 . 0.8600
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
O4 H4 O7 1_545 0.86 1.61 2.460(2) 171.8
O12 H12 O10 2_464 0.86 1.80 2.656(2) 171.1
