#------------------------------------------------------------------------------
#$Date: 2020-08-08 00:13:45 +0200 (Sat 08 de Aug de 2020) $
#$Revision: 255180 $
#$URL: svn://www.crystallography.net/cod/cif/4/00/36/4003650.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_4003650
loop_
_publ_author_name
'Gao, Hong-Qiang'
'Wei, Wen-Juan'
'Tan, Yu-Hui'
'Tang, Yun-Zhi'
_publ_section_title
;
 Phase Transition and Negative Thermal Expansion in Guanidinium
 Magnesium-Hypophosphite Hybrid Perovskite
;
_journal_name_full               'Chemistry of Materials'
_journal_paper_doi               10.1021/acs.chemmater.0c01654
_journal_year                    2020
_chemical_formula_moiety         '0.11(H24 Mg4 O24 P12), 0.44(C H6 N3)'
_chemical_formula_sum            'C2 H24 Mg2 N6 O12 P6'
_chemical_formula_weight         558.71
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                105.5997(8)
_cell_angle_beta                 91.0186(8)
_cell_angle_gamma                118.4961(9)
_cell_formula_units_Z            2
_cell_length_a                   8.99336(8)
_cell_length_b                   9.06691(8)
_cell_length_c                   15.65427(14)
_cell_measurement_reflns_used    9456
_cell_measurement_temperature    320(2)
_cell_measurement_theta_max      73.5190
_cell_measurement_theta_min      5.6630
_cell_volume                     1064.30(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.28b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      320(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10597
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.839
_diffrn_reflns_theta_min         5.666
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.897
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.51543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.28b (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.743
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_refine_diff_density_max         1.352
_refine_diff_density_min         -0.663
_refine_diff_density_rms         0.103
_refine_ls_extinction_coef       0.0156(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4156
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0449
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0599P)²+1.9900P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1166
_refine_ls_wR_factor_ref         0.1170
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4130
_reflns_number_total             4156
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            exp_38_09_320_00.cif
_cod_data_source_block           exp_38_09_320_00
_cod_original_cell_volume        1064.298(19)
_cod_database_code               4003650
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P2 P 0.87546(9) 0.21748(9) 0.15549(4) 0.02283(19) Uani 1 1 d . . . . .
P4 P 0.61507(9) -0.24108(10) 0.35628(5) 0.0291(2) Uani 1 1 d . . . . .
P5 P 0.33009(9) 0.35858(10) 0.15717(5) 0.0311(2) Uani 1 1 d . . . . .
P3 P 0.46987(10) 0.20739(10) 0.35586(5) 0.0317(2) Uani 1 1 d . . . . .
Mg3 Mg 0.0000 0.0000 0.0000 0.0144(2) Uani 1 2 d S . P . .
Mg1 Mg 0.73955(10) 0.48452(10) 0.25113(5) 0.0148(2) Uani 1 1 d . . . . .
Mg2 Mg 0.5000 0.0000 0.5000 0.0157(2) Uani 1 2 d S . P . .
O4 O 0.8343(2) 0.0609(2) 0.07507(12) 0.0229(4) Uani 1 1 d . . . . .
O3 O 0.7283(2) 0.2476(2) 0.17803(13) 0.0251(4) Uani 1 1 d . . . . .
O8 O 0.7572(2) -0.2787(2) 0.33367(13) 0.0249(4) Uani 1 1 d . . . . .
O9 O 0.5146(3) 0.4122(3) 0.17156(15) 0.0356(5) Uani 1 1 d . . . . .
O5 O 0.6089(3) 0.3722(3) 0.34352(15) 0.0347(5) Uani 1 1 d . . . . .
O7 O 0.6600(3) -0.0868(3) 0.43764(17) 0.0431(6) Uani 1 1 d . . . . .
O10 O 0.2056(3) 0.1742(3) 0.10312(15) 0.0391(6) Uani 1 1 d . . . . .
N3 N 0.9154(4) 0.2739(4) 0.39586(18) 0.0351(6) Uani 1 1 d . . . . .
H3C H 0.9313 0.3508 0.3694 0.042 Uiso 1 1 calc R U . . .
H3D H 0.8176 0.1784 0.3841 0.042 Uiso 1 1 calc R U . . .
N2 N 1.0175(3) 0.1791(3) 0.49166(17) 0.0289(5) Uani 1 1 d . . . . .
H2C H 0.9211 0.0816 0.4778 0.035 Uiso 1 1 calc R U . . .
H2D H 1.0991 0.1972 0.5298 0.035 Uiso 1 1 calc R U . . .
O6 O 0.5189(4) 0.1157(4) 0.4032(2) 0.0590(8) Uani 1 1 d . . . . .
N1 N 1.1921(4) 0.4485(3) 0.47297(19) 0.0375(6) Uani 1 1 d . . . . .
H1C H 1.2096 0.5264 0.4470 0.045 Uiso 1 1 calc R U . . .
H1D H 1.2730 0.4656 0.5112 0.045 Uiso 1 1 calc R U . . .
C1 C 1.0405(4) 0.3023(4) 0.45404(17) 0.0237(5) Uani 1 1 d . . . . .
O2 O 0.9795(2) 0.5598(2) 0.32167(13) 0.0231(4) Uani 1 1 d . . . . .
P1 P 1.15176(8) 0.72364(9) 0.33705(4) 0.02171(19) Uani 1 1 d . . . . .
O1 O 1.2792(2) 0.7657(2) 0.41567(13) 0.0262(4) Uani 1 1 d . . . . .
O11 O 0.0437(3) 0.1949(3) -0.05921(15) 0.0336(5) Uani 1 1 d . . . . .
P6 P 0.11677(10) 0.22902(10) -0.14133(5) 0.0275(2) Uani 1 1 d . . . . .
O12 O 0.1325(3) 0.3895(3) -0.15935(13) 0.0255(4) Uani 1 1 d . . . . .
N5 N 0.3791(3) -0.0538(4) 0.10485(18) 0.0364(6) Uani 1 1 d . . . . .
H5C H 0.4829 0.0284 0.1285 0.044 Uiso 1 1 calc R U . . .
H5D H 0.2947 -0.0389 0.1203 0.044 Uiso 1 1 calc R U . . .
N4 N 0.4774(3) -0.2282(4) 0.0202(2) 0.0374(6) Uani 1 1 d . . . . .
H4C H 0.5818 -0.1470 0.0433 0.045 Uiso 1 1 calc R U . . .
H4D H 0.4564 -0.3259 -0.0190 0.045 Uiso 1 1 calc R U . . .
N6 N 0.1889(3) -0.3314(3) 0.01186(17) 0.0298(5) Uani 1 1 d . . . . .
H6C H 0.1052 -0.3173 0.0296 0.036 Uiso 1 1 calc R U . . .
H6D H 0.1683 -0.4289 -0.0273 0.036 Uiso 1 1 calc R U . . .
C2 C 0.3493(4) -0.2030(4) 0.04477(18) 0.0250(6) Uani 1 1 d . . . . .
H2A H 0.947(5) 0.211(5) 0.221(2) 0.031(9) Uiso 1 1 d . . . . .
H2B H 1.011(5) 0.363(5) 0.144(2) 0.034(9) Uiso 1 1 d . . . . .
H1A H 1.133(5) 0.862(5) 0.346(3) 0.042(10) Uiso 1 1 d . . . . .
H5A H 0.307(7) 0.470(7) 0.121(4) 0.079(16) Uiso 1 1 d . . . . .
H1B H 1.222(4) 0.713(4) 0.270(2) 0.029(8) Uiso 1 1 d . . . . .
H4A H 0.480(5) -0.378(5) 0.364(3) 0.045(11) Uiso 1 1 d . . . . .
H6A H 0.017(6) 0.077(6) -0.211(3) 0.068(14) Uiso 1 1 d . . . . .
H4B H 0.549(6) -0.221(6) 0.289(3) 0.057(12) Uiso 1 1 d . . . . .
H3A H 0.371(6) 0.102(6) 0.280(3) 0.060(13) Uiso 1 1 d . . . . .
H6B H 0.261(6) 0.241(6) -0.140(3) 0.069(14) Uiso 1 1 d . . . . .
H5B H 0.280(5) 0.388(5) 0.234(3) 0.049(11) Uiso 1 1 d . . . . .
H3B H 0.353(7) 0.248(8) 0.401(4) 0.094(19) Uiso 1 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 0.0181 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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mg Mg 0.1719 0.1771 '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
O4 P2 O3 116.01(11) . . ?
O4 P2 H2A 109.6(16) . . ?
O3 P2 H2A 111.6(17) . . ?
O4 P2 H2B 107.9(15) . . ?
O3 P2 H2B 111.9(15) . . ?
H2A P2 H2B 98(2) . . ?
O7 P4 O8 115.87(12) . . ?
O7 P4 H4A 108.6(18) . . ?
O8 P4 H4A 112.2(18) . . ?
O7 P4 H4B 108(2) . . ?
O8 P4 H4B 112(2) . . ?
H4A P4 H4B 98(3) . . ?
O10 P5 O9 118.26(13) . . ?
O10 P5 H5A 108(2) . . ?
O9 P5 H5A 110(2) . . ?
O10 P5 H5B 106.9(19) . . ?
O9 P5 H5B 110.3(18) . . ?
H5A P5 H5B 102(3) . . ?
O6 P3 O5 117.85(16) . . ?
O6 P3 H3A 112(2) . . ?
O5 P3 H3A 110(2) . . ?
O6 P3 H3B 108(2) . . ?
O5 P3 H3B 108(2) . . ?
H3A P3 H3B 99(3) . . ?
O10 Mg3 O10 180.0 2 . ?
O10 Mg3 O11 87.51(10) 2 . ?
O10 Mg3 O11 92.49(10) . . ?
O10 Mg3 O11 92.49(10) 2 2 ?
O10 Mg3 O11 87.51(10) . 2 ?
O11 Mg3 O11 180.0 . 2 ?
O10 Mg3 O4 91.11(8) 2 2_655 ?
O10 Mg3 O4 88.89(8) . 2_655 ?
O11 Mg3 O4 89.99(8) . 2_655 ?
O11 Mg3 O4 90.01(8) 2 2_655 ?
O10 Mg3 O4 88.89(8) 2 1_455 ?
O10 Mg3 O4 91.11(8) . 1_455 ?
O11 Mg3 O4 90.01(8) . 1_455 ?
O11 Mg3 O4 89.99(8) 2 1_455 ?
O4 Mg3 O4 180.00(10) 2_655 1_455 ?
O5 Mg1 O9 92.26(10) . . ?
O5 Mg1 O12 176.41(9) . 2_665 ?
O9 Mg1 O12 86.31(9) . 2_665 ?
O5 Mg1 O3 91.34(9) . . ?
O9 Mg1 O3 90.42(9) . . ?
O12 Mg1 O3 91.95(8) 2_665 . ?
O5 Mg1 O2 92.62(9) . . ?
O9 Mg1 O2 174.76(9) . . ?
O12 Mg1 O2 88.94(8) 2_665 . ?
O3 Mg1 O2 87.54(8) . . ?
O5 Mg1 O8 85.80(9) . 1_565 ?
O9 Mg1 O8 92.86(9) . 1_565 ?
O12 Mg1 O8 90.99(8) 2_665 1_565 ?
O3 Mg1 O8 175.73(9) . 1_565 ?
O2 Mg1 O8 89.42(8) . 1_565 ?
O6 Mg2 O6 180.0 2_656 . ?
O6 Mg2 O7 93.21(13) 2_656 . ?
O6 Mg2 O7 86.79(13) . . ?
O6 Mg2 O7 86.79(13) 2_656 2_656 ?
O6 Mg2 O7 93.21(13) . 2_656 ?
O7 Mg2 O7 180.0 . 2_656 ?
O6 Mg2 O1 89.25(10) 2_656 2_766 ?
O6 Mg2 O1 90.75(10) . 2_766 ?
O7 Mg2 O1 89.71(8) . 2_766 ?
O7 Mg2 O1 90.28(8) 2_656 2_766 ?
O6 Mg2 O1 90.75(10) 2_656 1_445 ?
O6 Mg2 O1 89.25(10) . 1_445 ?
O7 Mg2 O1 90.29(8) . 1_445 ?
O7 Mg2 O1 89.72(8) 2_656 1_445 ?
O1 Mg2 O1 180.0 2_766 1_445 ?
P2 O4 Mg3 129.69(11) . 1_655 ?
P2 O3 Mg1 127.91(11) . . ?
P4 O8 Mg1 128.56(12) . 1_545 ?
P5 O9 Mg1 152.49(16) . . ?
P3 O5 Mg1 144.71(15) . . ?
P4 O7 Mg2 128.98(13) . . ?
P5 O10 Mg3 149.00(17) . . ?
C1 N3 H3C 120.0 . . ?
C1 N3 H3D 120.0 . . ?
H3C N3 H3D 120.0 . . ?
C1 N2 H2C 120.0 . . ?
C1 N2 H2D 120.0 . . ?
H2C N2 H2D 120.0 . . ?
P3 O6 Mg2 152.5(2) . . ?
C1 N1 H1C 120.0 . . ?
C1 N1 H1D 120.0 . . ?
H1C N1 H1D 120.0 . . ?
N3 C1 N1 120.9(3) . . ?
N3 C1 N2 119.7(3) . . ?
N1 C1 N2 119.4(3) . . ?
P1 O2 Mg1 130.59(12) . . ?
O1 P1 O2 115.97(11) . . ?
O1 P1 H1A 108.5(17) . . ?
O2 P1 H1A 110.2(17) . . ?
O1 P1 H1B 106.5(16) . . ?
O2 P1 H1B 110.5(16) . . ?
H1A P1 H1B 105(2) . . ?
P1 O1 Mg2 135.23(12) . 1_665 ?
P6 O11 Mg3 132.11(12) . . ?
O11 P6 O12 115.48(11) . . ?
O11 P6 H6A 106(2) . . ?
O12 P6 H6A 113(2) . . ?
O11 P6 H6B 112(2) . . ?
O12 P6 H6B 107(2) . . ?
H6A P6 H6B 103(3) . . ?
P6 O12 Mg1 129.96(12) . 2_665 ?
C2 N5 H5C 120.0 . . ?
C2 N5 H5D 120.0 . . ?
H5C N5 H5D 120.0 . . ?
C2 N4 H4C 120.0 . . ?
C2 N4 H4D 120.0 . . ?
H4C N4 H4D 120.0 . . ?
C2 N6 H6C 120.0 . . ?
C2 N6 H6D 120.0 . . ?
H6C N6 H6D 120.0 . . ?
N5 C2 N4 120.8(3) . . ?
N5 C2 N6 119.4(3) . . ?
N4 C2 N6 119.7(3) . . ?
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
P2 O4 1.5028(18) . ?
P2 O3 1.5036(19) . ?
P2 H2A 1.23(4) . ?
P2 H2B 1.37(4) . ?
P4 O7 1.492(2) . ?
P4 O8 1.4975(19) . ?
P4 H4A 1.30(4) . ?
P4 H4B 1.29(4) . ?
P5 O10 1.478(2) . ?
P5 O9 1.482(2) . ?
P5 H5A 1.38(5) . ?
P5 H5B 1.29(4) . ?
P3 O6 1.451(3) . ?
P3 O5 1.488(2) . ?
P3 H3A 1.29(5) . ?
P3 H3B 1.41(6) . ?
Mg3 O10 2.063(2) 2 ?
Mg3 O10 2.063(2) . ?
Mg3 O11 2.0900(19) . ?
Mg3 O11 2.0900(19) 2 ?
Mg3 O4 2.0985(17) 2_655 ?
Mg3 O4 2.0985(17) 1_455 ?
Mg1 O5 2.054(2) . ?
Mg1 O9 2.069(2) . ?
Mg1 O12 2.093(2) 2_665 ?
Mg1 O3 2.0977(19) . ?
Mg1 O2 2.1086(19) . ?
Mg1 O8 2.1166(19) 1_565 ?
Mg2 O6 2.029(2) 2_656 ?
Mg2 O6 2.029(2) . ?
Mg2 O7 2.088(2) . ?
Mg2 O7 2.088(2) 2_656 ?
Mg2 O1 2.1384(18) 2_766 ?
Mg2 O1 2.1384(18) 1_445 ?
O4 Mg3 2.0985(17) 1_655 ?
O8 Mg1 2.1165(19) 1_545 ?
N3 C1 1.312(4) . ?
N3 H3C 0.8600 . ?
N3 H3D 0.8600 . ?
N2 C1 1.332(4) . ?
N2 H2C 0.8600 . ?
N2 H2D 0.8600 . ?
N1 C1 1.324(4) . ?
N1 H1C 0.8600 . ?
N1 H1D 0.8600 . ?
O2 P1 1.5045(19) . ?
P1 O1 1.501(2) . ?
P1 H1A 1.32(4) . ?
P1 H1B 1.24(3) . ?
O1 Mg2 2.1384(18) 1_665 ?
O11 P6 1.493(2) . ?
P6 O12 1.4975(19) . ?
P6 H6A 1.36(5) . ?
P6 H6B 1.25(5) . ?
O12 Mg1 2.093(2) 2_665 ?
N5 C2 1.322(4) . ?
N5 H5C 0.8600 . ?
N5 H5D 0.8600 . ?
N4 C2 1.322(4) . ?
N4 H4C 0.8600 . ?
N4 H4D 0.8600 . ?
N6 C2 1.323(4) . ?
N6 H6C 0.8600 . ?
N6 H6D 0.8600 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 P2 O4 Mg3 163.75(13) . . . 1_655 ?
O4 P2 O3 Mg1 -156.95(13) . . . . ?
O7 P4 O8 Mg1 160.92(16) . . . 1_545 ?
O10 P5 O9 Mg1 -108.9(3) . . . . ?
O6 P3 O5 Mg1 110.9(3) . . . . ?
O8 P4 O7 Mg2 -174.16(17) . . . . ?
O9 P5 O10 Mg3 -131.4(3) . . . . ?
O5 P3 O6 Mg2 128.8(4) . . . . ?
Mg1 O2 P1 O1 158.85(13) . . . . ?
O2 P1 O1 Mg2 -156.15(15) . . . 1_665 ?
Mg3 O11 P6 O12 -177.88(16) . . . . ?
O11 P6 O12 Mg1 168.94(15) . . . 2_665 ?
