#------------------------------------------------------------------------------
#$Date: 2022-03-02 05:20:08 +0200 (Wed, 02 Mar 2022) $
#$Revision: 273207 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/56/64/1566474.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_1566474
loop_
_publ_author_name
'Ruth, Paul Niklas'
'Herbst-Irmer, Regine'
'Stalke, Dietmar'
_publ_section_title
;
 Hirshfeld atom refinement based on projector augmented wave densities
 with periodic boundary conditions
;
_journal_issue                   2
_journal_name_full               IUCrJ
_journal_page_first              286
_journal_page_last               297
_journal_paper_doi               10.1107/S2052252522001385
_journal_volume                  9
_journal_year                    2022
_chemical_formula_moiety         '2(C4 H3 O4), Mg, 6(H2 O)'
_chemical_formula_sum            'C8 H18 Mg O14'
_chemical_formula_weight         362.5363
_chemical_name_common            'Magnesium bis(hydrogen maleate) hexahydrate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           'xHARPY 0.1'
_cell_angle_alpha                90
_cell_angle_beta                 103.67(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.195(2)
_cell_length_b                   11.759(2)
_cell_length_c                   6.6206(13)
_cell_measurement_reflns_used    256398
_cell_measurement_temperature    14.9(2)
_cell_measurement_theta_max      36.06
_cell_measurement_theta_min      0.86
_cell_volume                     771.2(3)
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_publication_material  'xHARPY 0.1'
_computing_structure_refinement  'xHARPY 0.1'
_computing_structure_solution    'SHELXT-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      14.9(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  IPDSC-Q
_diffrn_measurement_method       'phi or omega oscillation scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.3532
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0088
_diffrn_reflns_Laue_measured_fraction_full 1.0
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            155955
_diffrn_reflns_point_group_measured_fraction_full 1.0
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        12.235
_diffrn_reflns_theta_max         26.199
_diffrn_reflns_theta_min         1.021
_diffrn_source                   SPring-8
_exptl_absorpt_coefficient_mu    0.049
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.561
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             380
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.7295
_refine_diff_density_min         -0.5218
_refine_diff_density_rms         0.0416
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   2.807
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         12589
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0178
_refine_ls_R_factor_gt           0.016
_refine_ls_shift/su_max          0.0
_refine_ls_shift/su_mean         0.0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[σ²(Fo²)]
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0318
_refine_ls_wR_factor_ref         0.0319
_reflns_Friedel_coverage         0.0
_reflns_number_gt                11713
_reflns_number_total             12589
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            fc5060.cif
_cod_data_source_block           HMa-Mg_xHARPy_BLYP
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1566474
loop_
_space_group_symop_operation_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_site_symmetry_order
O1 O 0.097285(7) 0.091977(5) 0.872516(12) 0.007951(9) Uani 1.0 1
H1 H -0.0209(5) 0.1131(3) 0.8315(7) 0.0302(11) Uani 1.0 1
O2 O -0.138422(7) 0.140628(6) 0.783343(13) 0.008934(10) Uani 1.0 1
O3 O 0.292801(7) 0.179949(6) 0.918646(12) 0.008245(10) Uani 1.0 1
O4 O -0.264799(7) 0.295336(6) 0.716995(12) 0.008762(10) Uani 1.0 1
C1 C 0.167196(8) 0.183301(7) 0.887289(13) 0.005566(10) Uani 1.0 1
C2 C 0.101217(9) 0.297797(7) 0.869509(14) 0.006412(10) Uani 1.0 1
H2 H 0.1743(3) 0.3668(2) 0.8987(5) 0.0238(7) Uani 1.0 1
C3 C -0.030929(9) 0.324910(7) 0.822511(14) 0.006607(10) Uani 1.0 1
H3 H -0.0575(3) 0.4141(2) 0.8140(6) 0.0260(7) Uani 1.0 1
C4 C -0.152887(8) 0.249361(7) 0.771166(13) 0.005825(10) Uani 1.0 1
Mg1 Mg 0.5 0.5 1.0 0.005164(7) Uani 1.0 2
O5 O 0.509574(7) 0.326545(6) 1.013045(13) 0.009167(10) Uani 1.0 1
H4 H 0.5858(4) 0.2842(3) 1.0868(7) 0.0275(9) Uani 1.0 1
H5 H 0.4329(3) 0.2774(3) 0.9780(6) 0.0270(8) Uani 1.0 1
O6 O 0.649659(9) 0.507815(7) 1.270025(13) 0.011822(13) Uani 1.0 1
H6 H 0.6606(4) 0.5603(3) 1.3810(6) 0.0324(9) Uani 1.0 1
H7 H 0.7278(4) 0.4595(3) 1.2942(6) 0.0287(8) Uani 1.0 1
O7 O 0.649468(9) 0.499689(6) 0.834776(13) 0.010132(11) Uani 1.0 1
H8 H 0.6599(4) 0.5589(3) 0.7414(6) 0.0276(8) Uani 1.0 1
H9 H 0.6825(4) 0.4301(3) 0.7880(6) 0.0253(8) Uani 1.0 1
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.005081(20) 0.005287(16) 0.01334(2) 0.000063(16) 0.001993(16) -0.000361(14)
H1 0.059(4) 0.0163(19) 0.020(2) -0.0055(17) 0.012(2) -0.006(2)
O2 0.00502(2) 0.005799(17) 0.01563(3) -0.000003(17) 0.001954(18) -0.000493(14)
O3 0.004416(20) 0.007058(18) 0.01305(2) 0.000186(17) 0.001792(16) -0.000299(14)
O4 0.00497(2) 0.007787(19) 0.01306(2) -0.000820(17) 0.001273(17) 0.000944(15)
C1 0.00421(2) 0.005320(20) 0.00725(2) 0.000075(17) 0.001391(17) -0.000138(16)
C2 0.00487(2) 0.00514(2) 0.00921(2) -0.000023(18) 0.001531(19) -0.000330(17)
H2 0.0173(14) 0.0172(14) 0.0356(18) -0.0055(13) 0.0032(12) -0.0078(11)
C3 0.00502(2) 0.005135(20) 0.00962(3) -0.000027(18) 0.001549(19) 0.000023(17)
H3 0.0231(15) 0.0127(13) 0.0410(19) 0.0024(13) 0.0043(14) 0.0062(11)
C4 0.00426(2) 0.00592(2) 0.00747(2) -0.000279(18) 0.001633(18) 0.000113(17)
Mg1 0.004035(16) 0.004873(14) 0.006761(15) -0.000374(11) 0.001516(12)
-0.000135(11)
O5 0.00646(2) 0.005601(17) 0.01483(3) 0.000272(17) 0.001296(18) -0.000262(14)
H4 0.0188(18) 0.0255(19) 0.035(2) -0.0000(17) -0.0009(15) 0.0053(14)
H5 0.0190(18) 0.0235(17) 0.039(2) -0.0006(17) 0.0069(16) -0.0095(14)
O6 0.00973(3) 0.01212(2) 0.01133(2) -0.004350(19) -0.002707(20) 0.004111(19)
H6 0.034(2) 0.035(2) 0.028(2) -0.0167(17) 0.0036(16) -0.0005(17)
H7 0.026(2) 0.029(2) 0.029(2) 0.0001(17) 0.0012(15) 0.0152(16)
O7 0.01077(3) 0.008366(20) 0.01395(3) 0.001589(18) 0.00784(2) 0.001669(17)
H8 0.034(2) 0.0250(18) 0.031(2) 0.0086(16) 0.0197(16) -0.0021(16)
H9 0.0235(19) 0.0262(17) 0.0299(20) -0.0045(16) 0.0125(15) 0.0029(15)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C -0.0005 0.0003 'HAR in xHARPy 0.1'
H H 0.0000 0.0000 'HAR in xHARPy 0.1'
Mg Mg 0.0085 0.0083 'HAR in xHARPy 0.1'
O O 0.0004 0.0013 'HAR in xHARPy 0.1'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C1 O1 H1 110.87(18)
C4 O2 H1 111.99(18)
O3 C1 O1 121.132(11)
O3 C1 C2 117.746(9)
O1 C1 C2 121.119(15)
C3 C2 C1 129.575(8)
C3 C2 H2 118.06(15)
C1 C2 H2 112.36(15)
C2 C3 C4 129.948(14)
C2 C3 H3 117.76(15)
C4 C3 H3 112.26(15)
O4 C4 O2 122.447(9)
O4 C4 C3 117.726(17)
O2 C4 C3 119.825(13)
O5 Mg1 O6 89.407(4)
O5 Mg1 O7 89.245(3)
O6 Mg1 O7 88.395(18)
Mg1 O5 H4 124.6(2)
Mg1 O5 H5 124.4(2)
H4 O5 H5 109.2(4)
Mg1 O6 H6 129.1(2)
Mg1 O6 H7 122.3(2)
H6 O6 H7 108.3(3)
Mg1 O7 H8 123.3(2)
Mg1 O7 H9 121.8(2)
H8 O7 H9 108.1(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C1 1.2798(2)
O1 H1 1.196(5)
O2 C4 1.2874(2)
O2 H1 1.209(5)
O3 C1 1.2485(3)
O4 C4 1.2366(3)
C1 C2 1.4972(2)
C2 C3 1.3474(3)
C2 H2 1.088(3)
C3 C4 1.5003(3)
C3 H3 1.081(3)
Mg1 O5 2.0428(4)
Mg1 O6 2.0599(7)
Mg1 O7 2.0752(5)
O5 H4 0.955(3)
O5 H5 0.955(3)
O6 H6 0.945(4)
O6 H7 0.960(3)
O7 H8 0.953(4)
O7 H9 0.964(4)
