#------------------------------------------------------------------------------
#$Date: 2020-08-08 01:14:31 +0300 (Sat, 08 Aug 2020) $
#$Revision: 255183 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/36/4003653.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_4003653
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                105.5887(8)
_cell_angle_beta                 90.9969(7)
_cell_angle_gamma                118.5040(9)
_cell_formula_units_Z            2
_cell_length_a                   8.98838(8)
_cell_length_b                   9.06949(8)
_cell_length_c                   15.62933(14)
_cell_measurement_reflns_used    9481
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      73.6790
_cell_measurement_theta_min      5.6730
_cell_volume                     1062.39(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      300(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.959
_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  0.0312
_diffrn_reflns_av_unetI/netI     0.0308
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.959
_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            10574
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.927
_diffrn_reflns_theta_min         5.667
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.908
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47114
_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    1.747
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_refine_diff_density_max         1.406
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.0157(6)
_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   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4152
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0420
_refine_ls_R_factor_gt           0.0417
_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)+(0.0517P)²+1.7724P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1081
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4127
_reflns_number_total             4152
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            exp_38_07_300_00.cif
_cod_data_source_block           exp_38_07_300_00
_cod_original_cell_volume        1062.391(19)
_cod_database_code               4003653
_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
P1 P 0.15190(8) 0.72278(8) 0.33697(4) 0.01996(17) Uani 1 1 d . . . . .
O2 O -0.0206(2) 0.5590(2) 0.32175(12) 0.0212(4) Uani 1 1 d . . . . .
O1 O 0.2795(2) 0.7652(2) 0.41587(12) 0.0244(4) Uani 1 1 d . . . . .
Mg1 Mg -0.26064(9) 0.48420(9) 0.25119(5) 0.01373(19) Uani 1 1 d . . . . .
O9 O -0.4854(2) 0.4125(3) 0.17150(14) 0.0326(5) Uani 1 1 d . . . . .
P5 P -0.67037(8) 0.35847(9) 0.15727(5) 0.02858(19) Uani 1 1 d . . . . .
O10 O -0.7952(3) 0.1729(3) 0.10399(14) 0.0349(5) Uani 1 1 d . . . . .
Mg3 Mg -1.0000 0.0000 0.0000 0.0135(2) Uani 1 2 d S . P . .
O5 O -0.3919(3) 0.3728(3) 0.34382(14) 0.0317(5) Uani 1 1 d . . . . .
P3 P -0.53088(9) 0.20736(9) 0.35605(5) 0.02867(19) Uani 1 1 d . . . . .
O6 O -0.4802(3) 0.1130(3) 0.40143(18) 0.0510(7) Uani 1 1 d . . . . .
N3 N -0.0856(3) 0.2736(3) 0.39613(16) 0.0318(5) Uani 1 1 d . . . . .
H3C H -0.0696 0.3508 0.3698 0.038 Uiso 1 1 calc R U . . .
H3D H -0.1836 0.1782 0.3843 0.038 Uiso 1 1 calc R U . . .
N2 N 0.0166(3) 0.1784(3) 0.49192(16) 0.0264(5) Uani 1 1 d . . . . .
H2C H -0.0799 0.0809 0.4781 0.032 Uiso 1 1 calc R U . . .
H2D H 0.0983 0.1962 0.5300 0.032 Uiso 1 1 calc R U . . .
N1 N 0.1914(3) 0.4481(3) 0.47326(18) 0.0343(6) Uani 1 1 d . . . . .
H1C H 0.2087 0.5260 0.4473 0.041 Uiso 1 1 calc R U . . .
H1D H 0.2725 0.4651 0.5114 0.041 Uiso 1 1 calc R U . . .
C1 C 0.0396(3) 0.3015(3) 0.45434(16) 0.0218(5) Uani 1 1 d . . . . .
Mg2 Mg -0.5000 0.0000 0.5000 0.0146(2) Uani 1 2 d S . P . .
O7 O -0.3402(3) -0.0884(3) 0.43894(15) 0.0384(5) Uani 1 1 d . . . . .
P4 P -0.38511(8) -0.24180(9) 0.35677(5) 0.02692(19) Uani 1 1 d . . . . .
O8 O -0.2427(2) -0.2788(2) 0.33372(12) 0.0231(4) Uani 1 1 d . . . . .
C2 C -0.6512(3) -0.2031(3) 0.04456(17) 0.0230(5) Uani 1 1 d . . . . .
N6 N -0.8119(3) -0.3315(3) 0.01133(16) 0.0270(5) Uani 1 1 d . . . . .
H6C H -0.8325 -0.4308 -0.0258 0.032 Uiso 1 1 calc R U . . .
H6D H -0.8957 -0.3154 0.0269 0.032 Uiso 1 1 calc R U . . .
N4 N -0.5230(3) -0.2288(3) 0.02022(18) 0.0342(6) Uani 1 1 d . . . . .
H4C H -0.4186 -0.1479 0.0436 0.041 Uiso 1 1 calc R U . . .
H4D H -0.5442 -0.3265 -0.0190 0.041 Uiso 1 1 calc R U . . .
N5 N -0.6212(3) -0.0536(3) 0.10479(17) 0.0335(6) Uani 1 1 d . . . . .
H5C H -0.5173 0.0283 0.1286 0.040 Uiso 1 1 calc R U . . .
H5D H -0.7056 -0.0384 0.1201 0.040 Uiso 1 1 calc R U . . .
O3 O -0.2723(2) 0.2470(2) 0.17819(12) 0.0231(4) Uani 1 1 d . . . . .
P2 P -0.12514(8) 0.21670(8) 0.15567(4) 0.02083(17) Uani 1 1 d . . . . .
O4 O -0.1662(2) 0.0602(2) 0.07499(12) 0.0209(4) Uani 1 1 d . . . . .
P6 P -0.88275(9) 0.22955(9) -0.14125(5) 0.02537(19) Uani 1 1 d . . . . .
O12 O -0.8678(2) 0.3898(2) -0.15940(12) 0.0234(4) Uani 1 1 d . . . . .
O11 O -0.9547(3) 0.1962(3) -0.05847(14) 0.0304(5) Uani 1 1 d . . . . .
H2A H 0.009(4) 0.360(4) 0.144(2) 0.031(8) Uiso 1 1 d . . . . .
H2B H -0.057(5) 0.208(5) 0.223(2) 0.035(9) Uiso 1 1 d . . . . .
H3A H -0.646(6) 0.242(6) 0.399(3) 0.068(14) Uiso 1 1 d . . . . .
H1A H 0.134(4) 0.863(5) 0.346(2) 0.034(9) Uiso 1 1 d . . . . .
H5A H -0.694(6) 0.468(6) 0.123(3) 0.062(13) Uiso 1 1 d . . . . .
H1B H 0.222(4) 0.712(4) 0.269(2) 0.030(8) Uiso 1 1 d . . . . .
H4A H -0.520(5) -0.381(5) 0.366(2) 0.042(10) Uiso 1 1 d . . . . .
H6A H -0.986(6) 0.080(6) -0.211(3) 0.066(13) Uiso 1 1 d . . . . .
H3B H -0.628(5) 0.100(5) 0.279(3) 0.051(11) Uiso 1 1 d . . . . .
H4B H -0.447(6) -0.218(6) 0.290(3) 0.065(13) Uiso 1 1 d . . . . .
H6B H -0.740(6) 0.242(6) -0.141(3) 0.057(12) Uiso 1 1 d . . . . .
H5B H -0.717(5) 0.393(5) 0.235(3) 0.049(11) 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'
Mg Mg 0.1719 0.1771 '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'
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
O1 P1 O2 115.97(10) . . ?
O1 P1 H1A 108.2(15) . . ?
O2 P1 H1A 110.7(15) . . ?
O1 P1 H1B 106.5(15) . . ?
O2 P1 H1B 110.7(15) . . ?
H1A P1 H1B 104(2) . . ?
P1 O2 Mg1 130.50(11) . . ?
P1 O1 Mg2 135.06(11) . 1_665 ?
O5 Mg1 O9 92.20(9) . . ?
O5 Mg1 O12 176.18(8) . 2_465 ?
O9 Mg1 O12 86.31(9) . 2_465 ?
O5 Mg1 O3 91.46(8) . . ?
O9 Mg1 O3 90.50(8) . . ?
O12 Mg1 O3 92.08(7) 2_465 . ?
O5 Mg1 O2 92.76(8) . . ?
O9 Mg1 O2 174.68(8) . . ?
O12 Mg1 O2 88.86(8) 2_465 . ?
O3 Mg1 O2 87.46(7) . . ?
O5 Mg1 O8 85.66(8) . 1_565 ?
O9 Mg1 O8 92.80(8) . 1_565 ?
O12 Mg1 O8 90.89(7) 2_465 1_565 ?
O3 Mg1 O8 175.70(8) . 1_565 ?
O2 Mg1 O8 89.49(7) . 1_565 ?
P5 O9 Mg1 152.29(15) . . ?
O10 P5 O9 118.18(12) . . ?
O10 P5 H5A 109.5(19) . . ?
O9 P5 H5A 110.4(19) . . ?
O10 P5 H5B 108.2(18) . . ?
O9 P5 H5B 109.3(18) . . ?
H5A P5 H5B 100(3) . . ?
P5 O10 Mg3 148.04(15) . . ?
O10 Mg3 O10 180.0 2_355 . ?
O10 Mg3 O11 92.49(9) 2_355 2_355 ?
O10 Mg3 O11 87.51(9) . 2_355 ?
O10 Mg3 O11 87.51(9) 2_355 . ?
O10 Mg3 O11 92.49(9) . . ?
O11 Mg3 O11 180.0 2_355 . ?
O10 Mg3 O4 88.96(8) 2_355 1_455 ?
O10 Mg3 O4 91.04(8) . 1_455 ?
O11 Mg3 O4 89.96(7) 2_355 1_455 ?
O11 Mg3 O4 90.04(7) . 1_455 ?
O10 Mg3 O4 91.04(8) 2_355 2_455 ?
O10 Mg3 O4 88.96(8) . 2_455 ?
O11 Mg3 O4 90.04(7) 2_355 2_455 ?
O11 Mg3 O4 89.96(7) . 2_455 ?
O4 Mg3 O4 180.00(9) 1_455 2_455 ?
P3 O5 Mg1 144.46(13) . . ?
O6 P3 O5 117.68(14) . . ?
O6 P3 H3A 109(2) . . ?
O5 P3 H3A 109(2) . . ?
O6 P3 H3B 109.2(18) . . ?
O5 P3 H3B 110.1(18) . . ?
H3A P3 H3B 100(3) . . ?
P3 O6 Mg2 150.27(19) . . ?
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 . . ?
C1 N1 H1C 120.0 . . ?
C1 N1 H1D 120.0 . . ?
H1C N1 H1D 120.0 . . ?
N3 C1 N1 120.7(3) . . ?
N3 C1 N2 119.8(2) . . ?
N1 C1 N2 119.4(2) . . ?
O6 Mg2 O6 180.00(17) . 2_456 ?
O6 Mg2 O7 93.26(11) . 2_456 ?
O6 Mg2 O7 86.74(11) 2_456 2_456 ?
O6 Mg2 O7 86.74(11) . . ?
O6 Mg2 O7 93.27(11) 2_456 . ?
O7 Mg2 O7 180.0 2_456 . ?
O6 Mg2 O1 89.05(9) . 1_445 ?
O6 Mg2 O1 90.95(9) 2_456 1_445 ?
O7 Mg2 O1 89.84(7) 2_456 1_445 ?
O7 Mg2 O1 90.16(7) . 1_445 ?
O6 Mg2 O1 90.95(9) . 2_566 ?
O6 Mg2 O1 89.05(9) 2_456 2_566 ?
O7 Mg2 O1 90.16(7) 2_456 2_566 ?
O7 Mg2 O1 89.84(7) . 2_566 ?
O1 Mg2 O1 180.0 1_445 2_566 ?
P4 O7 Mg2 128.75(12) . . ?
O7 P4 O8 115.77(11) . . ?
O7 P4 H4A 108.2(16) . . ?
O8 P4 H4A 111.5(16) . . ?
O7 P4 H4B 108(2) . . ?
O8 P4 H4B 111(2) . . ?
H4A P4 H4B 101(3) . . ?
P4 O8 Mg1 128.41(11) . 1_545 ?
N4 C2 N5 120.9(3) . . ?
N4 C2 N6 119.6(2) . . ?
N5 C2 N6 119.4(2) . . ?
C2 N6 H6C 120.0 . . ?
C2 N6 H6D 120.0 . . ?
H6C N6 H6D 120.0 . . ?
C2 N4 H4C 120.0 . . ?
C2 N4 H4D 120.0 . . ?
H4C N4 H4D 120.0 . . ?
C2 N5 H5C 120.0 . . ?
C2 N5 H5D 120.0 . . ?
H5C N5 H5D 120.0 . . ?
P2 O3 Mg1 127.88(11) . . ?
O3 P2 O4 116.02(10) . . ?
O3 P2 H2A 111.9(14) . . ?
O4 P2 H2A 107.8(14) . . ?
O3 P2 H2B 109.8(16) . . ?
O4 P2 H2B 110.1(16) . . ?
H2A P2 H2B 100(2) . . ?
P2 O4 Mg3 129.57(11) . 1_655 ?
O11 P6 O12 115.37(10) . . ?
O11 P6 H6A 105.7(19) . . ?
O12 P6 H6A 111.3(19) . . ?
O11 P6 H6B 112(2) . . ?
O12 P6 H6B 107(2) . . ?
H6A P6 H6B 104(3) . . ?
P6 O12 Mg1 129.76(11) . 2_465 ?
P6 O11 Mg3 131.96(11) . . ?
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
P1 O1 1.5031(19) . ?
P1 O2 1.5055(18) . ?
P1 H1A 1.32(3) . ?
P1 H1B 1.25(3) . ?
O2 Mg1 2.1091(18) . ?
O1 Mg2 2.1372(17) 1_665 ?
Mg1 O5 2.054(2) . ?
Mg1 O9 2.069(2) . ?
Mg1 O12 2.0920(19) 2_465 ?
Mg1 O3 2.0984(18) . ?
Mg1 O8 2.1171(18) 1_565 ?
O9 P5 1.485(2) . ?
P5 O10 1.482(2) . ?
P5 H5A 1.34(5) . ?
P5 H5B 1.29(4) . ?
O10 Mg3 2.0641(19) . ?
Mg3 O10 2.0641(19) 2_355 ?
Mg3 O11 2.0885(18) 2_355 ?
Mg3 O11 2.0885(18) . ?
Mg3 O4 2.0978(16) 1_455 ?
Mg3 O4 2.0978(16) 2_455 ?
O5 P3 1.490(2) . ?
P3 O6 1.459(2) . ?
P3 H3A 1.35(5) . ?
P3 H3B 1.29(4) . ?
O6 Mg2 2.035(2) . ?
N3 C1 1.314(4) . ?
N3 H3C 0.8600 . ?
N3 H3D 0.8600 . ?
N2 C1 1.331(3) . ?
N2 H2C 0.8600 . ?
N2 H2D 0.8600 . ?
N1 C1 1.327(4) . ?
N1 H1C 0.8600 . ?
N1 H1D 0.8600 . ?
Mg2 O6 2.035(2) 2_456 ?
Mg2 O7 2.0866(19) 2_456 ?
Mg2 O7 2.0866(19) . ?
Mg2 O1 2.1372(17) 1_445 ?
Mg2 O1 2.1372(17) 2_566 ?
O7 P4 1.4944(19) . ?
P4 O8 1.4973(18) . ?
P4 H4A 1.31(4) . ?
P4 H4B 1.29(5) . ?
O8 Mg1 2.1172(18) 1_545 ?
C2 N4 1.323(4) . ?
C2 N5 1.324(3) . ?
C2 N6 1.325(3) . ?
N6 H6C 0.8600 . ?
N6 H6D 0.8600 . ?
N4 H4C 0.8600 . ?
N4 H4D 0.8600 . ?
N5 H5C 0.8600 . ?
N5 H5D 0.8600 . ?
O3 P2 1.5029(18) . ?
P2 O4 1.5041(17) . ?
P2 H2A 1.35(3) . ?
P2 H2B 1.25(4) . ?
O4 Mg3 2.0978(16) 1_655 ?
P6 O11 1.4955(19) . ?
P6 O12 1.4990(18) . ?
P6 H6A 1.36(5) . ?
P6 H6B 1.24(4) . ?
O12 Mg1 2.0921(18) 2_465 ?
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
O1 P1 O2 Mg1 158.72(12) . . . . ?
O2 P1 O1 Mg2 -155.98(14) . . . 1_665 ?
Mg1 O9 P5 O10 -107.7(3) . . . . ?
O9 P5 O10 Mg3 -130.4(2) . . . . ?
Mg1 O5 P3 O6 108.4(3) . . . . ?
O5 P3 O6 Mg2 127.0(3) . . . . ?
Mg2 O7 P4 O8 -175.74(15) . . . . ?
O7 P4 O8 Mg1 160.11(15) . . . 1_545 ?
Mg1 O3 P2 O4 -156.73(12) . . . . ?
O3 P2 O4 Mg3 163.67(12) . . . 1_655 ?
O11 P6 O12 Mg1 168.30(14) . . . 2_465 ?
O12 P6 O11 Mg3 -178.87(15) . . . . ?
