#------------------------------------------------------------------------------
#$Date: 2020-08-08 01:12:27 +0300 (Sat, 08 Aug 2020) $
#$Revision: 255175 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/36/4003645.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_4003645
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                105.5831(8)
_cell_angle_beta                 90.9628(9)
_cell_angle_gamma                118.5074(10)
_cell_formula_units_Z            2
_cell_length_a                   8.98497(10)
_cell_length_b                   9.07444(7)
_cell_length_c                   15.61097(16)
_cell_measurement_reflns_used    9385
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      73.5970
_cell_measurement_theta_min      5.6720
_cell_volume                     1061.45(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      290(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  0.0232
_diffrn_reflns_av_unetI/netI     0.0222
_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            10572
_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         73.785
_diffrn_reflns_theta_min         5.665
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.913
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.46227
_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    1.748
_exptl_crystal_description       block
_exptl_crystal_F_000             576.0
_refine_diff_density_max         1.342
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0266(8)
_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   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4146
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0511P)²+1.4475P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0977
_refine_ls_wR_factor_ref         0.0979
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4129
_reflns_number_total             4146
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            exp_38_01_290_00.cif
_cod_data_source_block           exp_38_01_290_00
_cod_database_code               4003645
_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 1.15186(7) 0.72168(7) 0.83677(4) 0.01726(16) Uani 1 1 d . . . . .
P2 P 0.87388(7) 0.21548(7) 0.65590(4) 0.01763(16) Uani 1 1 d . . . . .
P3 P 0.46842(8) 0.20738(8) 0.85634(4) 0.02440(17) Uani 1 1 d . . . . .
P5 P 0.32905(7) 0.35814(8) 0.65732(4) 0.02437(17) Uani 1 1 d . . . . .
P4 P 0.61485(7) -0.24242(8) 0.85725(4) 0.02370(17) Uani 1 1 d . . . . .
Mg1 Mg 0.73899(8) 0.48371(9) 0.75121(4) 0.01188(17) Uani 1 1 d . . . . .
Mg3 Mg 0.0000 0.0000 0.5000 0.0117(2) Uani 1 2 d S . P . .
Mg2 Mg 0.5000 0.0000 1.0000 0.0128(2) Uani 1 2 d S . P . .
O4 O 0.8328(2) 0.0593(2) 0.57476(10) 0.0185(3) Uani 1 1 d . . . . .
O1 O 1.2797(2) 0.7644(2) 0.91592(11) 0.0215(3) Uani 1 1 d . . . . .
O2 O 0.97918(19) 0.5582(2) 0.82173(11) 0.0188(3) Uani 1 1 d . . . . .
O8 O 0.7578(2) -0.2791(2) 0.83368(11) 0.0204(3) Uani 1 1 d . . . . .
O3 O 0.7268(2) 0.2464(2) 0.67836(11) 0.0204(3) Uani 1 1 d . . . . .
O7 O 0.6600(2) -0.0896(2) 0.94023(13) 0.0323(4) Uani 1 1 d . . . . .
O9 O 0.5145(2) 0.4129(2) 0.67130(12) 0.0285(4) Uani 1 1 d . . . . .
O5 O 0.6072(2) 0.3731(2) 0.84416(12) 0.0282(4) Uani 1 1 d . . . . .
O10 O 0.2038(2) 0.1716(2) 0.60478(12) 0.0297(4) Uani 1 1 d . . . . .
O6 O 0.5205(3) 0.1110(3) 0.90022(15) 0.0422(5) Uani 1 1 d . . . . .
N3 N 0.9133(3) 0.2734(3) 0.89644(14) 0.0279(5) Uani 1 1 d . . . . .
H3C H 0.9295 0.3505 0.8700 0.034 Uiso 1 1 calc R U . . .
H3D H 0.8151 0.1783 0.8848 0.034 Uiso 1 1 calc R U . . .
N2 N 1.0160(3) 0.1782(3) 0.99233(14) 0.0226(4) Uani 1 1 d . . . . .
H2C H 0.9193 0.0809 0.9786 0.027 Uiso 1 1 calc R U . . .
H2D H 1.0978 0.1959 1.0304 0.027 Uiso 1 1 calc R U . . .
N1 N 1.1912(3) 0.4473(3) 0.97326(15) 0.0302(5) Uani 1 1 d . . . . .
H1C H 1.2084 0.5251 0.9472 0.036 Uiso 1 1 calc R U . . .
H1D H 1.2724 0.4643 1.0114 0.036 Uiso 1 1 calc R U . . .
C1 C 1.0390(3) 0.3011(3) 0.95472(14) 0.0191(4) Uani 1 1 d . . . . .
O11 O 0.0469(2) 0.1976(2) 0.44218(12) 0.0257(4) Uani 1 1 d . . . . .
N5 N 0.3783(3) -0.0539(3) 0.60454(15) 0.0289(5) Uani 1 1 d . . . . .
H5C H 0.2941 -0.0402 0.6218 0.035 Uiso 1 1 calc R U . . .
H5D H 0.4825 0.0296 0.6264 0.035 Uiso 1 1 calc R U . . .
P6 P 0.11794(8) 0.23036(8) 0.35892(4) 0.02206(17) Uani 1 1 d . . . . .
N6 N 0.1871(2) -0.3317(3) 0.51091(14) 0.0226(4) Uani 1 1 d . . . . .
H6C H 0.1032 -0.3174 0.5284 0.027 Uiso 1 1 calc R U . . .
H6D H 0.1666 -0.4291 0.4718 0.027 Uiso 1 1 calc R U . . .
N4 N 0.4764(3) -0.2295(3) 0.52014(16) 0.0298(5) Uani 1 1 d . . . . .
H4C H 0.4553 -0.3291 0.4830 0.036 Uiso 1 1 calc R U . . .
H4D H 0.5810 -0.1467 0.5416 0.036 Uiso 1 1 calc R U . . .
C2 C 0.3477(3) -0.2036(3) 0.54427(15) 0.0193(4) Uani 1 1 d . . . . .
O12 O 0.1322(2) 0.3905(2) 0.34071(11) 0.0202(3) Uani 1 1 d . . . . .
H2A H 0.939(4) 0.203(4) 0.725(2) 0.030(8) Uiso 1 1 d . . . . .
H1A H 1.134(4) 0.861(4) 0.844(2) 0.026(7) Uiso 1 1 d . . . . .
H5A H 0.305(5) 0.469(5) 0.624(3) 0.055(11) Uiso 1 1 d . . . . .
H1B H 1.223(4) 0.711(4) 0.766(2) 0.027(7) Uiso 1 1 d . . . . .
H3A H 0.363(5) 0.247(5) 0.904(3) 0.061(12) Uiso 1 1 d . . . . .
H2B H 1.007(4) 0.358(4) 0.643(2) 0.028(8) Uiso 1 1 d . . . . .
H6A H 0.014(5) 0.081(5) 0.292(3) 0.059(11) Uiso 1 1 d . . . . .
H4A H 0.554(6) -0.219(6) 0.789(3) 0.064(12) Uiso 1 1 d . . . . .
H4B H 0.479(4) -0.381(5) 0.866(2) 0.039(9) Uiso 1 1 d . . . . .
H3B H 0.369(5) 0.099(5) 0.778(2) 0.049(10) Uiso 1 1 d . . . . .
H5B H 0.281(4) 0.389(4) 0.734(2) 0.040(9) Uiso 1 1 d . . . . .
H6B H 0.266(5) 0.246(5) 0.361(3) 0.058(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'
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
O1 P1 O2 115.99(9) . . ?
O1 P1 H1A 109.0(13) . . ?
O2 P1 H1A 110.7(13) . . ?
O1 P1 H1B 107.3(13) . . ?
O2 P1 H1B 110.5(14) . . ?
H1A P1 H1B 102.4(19) . . ?
O3 P2 O4 116.05(9) . . ?
O3 P2 H2A 109.1(14) . . ?
O4 P2 H2A 109.8(14) . . ?
O3 P2 H2B 111.8(13) . . ?
O4 P2 H2B 107.1(13) . . ?
H2A P2 H2B 102.2(19) . . ?
O6 P3 O5 117.51(12) . . ?
O6 P3 H3A 108.5(18) . . ?
O5 P3 H3A 107.9(18) . . ?
O6 P3 H3B 109.4(16) . . ?
O5 P3 H3B 109.7(16) . . ?
H3A P3 H3B 103(2) . . ?
O10 P5 O9 118.25(11) . . ?
O10 P5 H5A 110.4(17) . . ?
O9 P5 H5A 110.4(17) . . ?
O10 P5 H5B 106.7(15) . . ?
O9 P5 H5B 109.6(15) . . ?
H5A P5 H5B 100(2) . . ?
O7 P4 O8 115.70(10) . . ?
O7 P4 H4A 109.1(19) . . ?
O8 P4 H4A 109.7(19) . . ?
O7 P4 H4B 107.8(15) . . ?
O8 P4 H4B 112.1(15) . . ?
H4A P4 H4B 101(2) . . ?
O5 Mg1 O9 92.26(8) . . ?
O5 Mg1 O12 176.02(7) . 2_666 ?
O9 Mg1 O12 86.21(7) . 2_666 ?
O5 Mg1 O3 91.53(7) . . ?
O9 Mg1 O3 90.54(7) . . ?
O12 Mg1 O3 92.16(7) 2_666 . ?
O5 Mg1 O2 92.87(7) . . ?
O9 Mg1 O2 174.53(7) . . ?
O12 Mg1 O2 88.78(7) 2_666 . ?
O3 Mg1 O2 87.46(7) . . ?
O5 Mg1 O8 85.60(7) . 1_565 ?
O9 Mg1 O8 92.83(7) . 1_565 ?
O12 Mg1 O8 90.80(7) 2_666 1_565 ?
O3 Mg1 O8 175.65(7) . 1_565 ?
O2 Mg1 O8 89.43(7) . 1_565 ?
O10 Mg3 O10 180.0 . 2_556 ?
O10 Mg3 O11 92.49(8) . . ?
O10 Mg3 O11 87.51(8) 2_556 . ?
O10 Mg3 O11 87.51(8) . 2_556 ?
O10 Mg3 O11 92.49(8) 2_556 2_556 ?
O11 Mg3 O11 180.0 . 2_556 ?
O10 Mg3 O4 88.98(7) . 2_656 ?
O10 Mg3 O4 91.02(7) 2_556 2_656 ?
O11 Mg3 O4 89.91(6) . 2_656 ?
O11 Mg3 O4 90.09(6) 2_556 2_656 ?
O10 Mg3 O4 91.02(7) . 1_455 ?
O10 Mg3 O4 88.98(7) 2_556 1_455 ?
O11 Mg3 O4 90.09(6) . 1_455 ?
O11 Mg3 O4 89.91(6) 2_556 1_455 ?
O4 Mg3 O4 180.0 2_656 1_455 ?
O6 Mg2 O6 180.00(16) 2_657 . ?
O6 Mg2 O7 86.85(9) 2_657 2_657 ?
O6 Mg2 O7 93.15(9) . 2_657 ?
O6 Mg2 O7 93.15(9) 2_657 . ?
O6 Mg2 O7 86.85(9) . . ?
O7 Mg2 O7 180.0 2_657 . ?
O6 Mg2 O1 88.97(8) 2_657 2_767 ?
O6 Mg2 O1 91.03(8) . 2_767 ?
O7 Mg2 O1 90.06(7) 2_657 2_767 ?
O7 Mg2 O1 89.94(7) . 2_767 ?
O6 Mg2 O1 91.03(8) 2_657 1_445 ?
O6 Mg2 O1 88.97(8) . 1_445 ?
O7 Mg2 O1 89.94(7) 2_657 1_445 ?
O7 Mg2 O1 90.06(7) . 1_445 ?
O1 Mg2 O1 180.0 2_767 1_445 ?
P2 O4 Mg3 129.39(9) . 1_655 ?
P1 O1 Mg2 134.89(10) . 1_665 ?
P1 O2 Mg1 130.45(10) . . ?
P4 O8 Mg1 128.20(10) . 1_545 ?
P2 O3 Mg1 127.87(9) . . ?
P4 O7 Mg2 128.41(11) . . ?
P5 O9 Mg1 151.97(13) . . ?
P3 O5 Mg1 144.25(12) . . ?
P5 O10 Mg3 147.20(13) . . ?
P3 O6 Mg2 148.51(16) . . ?
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 120.6(2) . . ?
N3 C1 N2 119.9(2) . . ?
N1 C1 N2 119.5(2) . . ?
P6 O11 Mg3 131.83(10) . . ?
C2 N5 H5C 120.0 . . ?
C2 N5 H5D 120.0 . . ?
H5C N5 H5D 120.0 . . ?
O11 P6 O12 115.24(9) . . ?
O11 P6 H6A 104.5(17) . . ?
O12 P6 H6A 112.4(17) . . ?
O11 P6 H6B 111.3(18) . . ?
O12 P6 H6B 107.2(18) . . ?
H6A P6 H6B 106(3) . . ?
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 . . ?
N6 C2 N5 119.7(2) . . ?
N6 C2 N4 119.7(2) . . ?
N5 C2 N4 120.6(2) . . ?
P6 O12 Mg1 129.50(10) . 2_666 ?
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 1.5056(17) . ?
P1 O2 1.5057(16) . ?
P1 H1A 1.33(3) . ?
P1 H1B 1.30(3) . ?
P2 O3 1.5049(16) . ?
P2 O4 1.5068(15) . ?
P2 H2A 1.28(3) . ?
P2 H2B 1.35(3) . ?
P3 O6 1.468(2) . ?
P3 O5 1.4912(18) . ?
P3 H3A 1.34(4) . ?
P3 H3B 1.32(4) . ?
P5 O10 1.4862(18) . ?
P5 O9 1.4871(17) . ?
P5 H5A 1.34(4) . ?
P5 H5B 1.29(3) . ?
P4 O7 1.4987(17) . ?
P4 O8 1.5013(16) . ?
P4 H4A 1.30(4) . ?
P4 H4B 1.31(3) . ?
Mg1 O5 2.0545(18) . ?
Mg1 O9 2.0697(18) . ?
Mg1 O12 2.0921(16) 2_666 ?
Mg1 O3 2.0973(16) . ?
Mg1 O2 2.1106(16) . ?
Mg1 O8 2.1156(17) 1_565 ?
Mg3 O10 2.0647(17) . ?
Mg3 O10 2.0647(17) 2_556 ?
Mg3 O11 2.0900(16) . ?
Mg3 O11 2.0900(16) 2_556 ?
Mg3 O4 2.0976(15) 2_656 ?
Mg3 O4 2.0976(15) 1_455 ?
Mg2 O6 2.0369(19) 2_657 ?
Mg2 O6 2.0370(19) . ?
Mg2 O7 2.0857(17) 2_657 ?
Mg2 O7 2.0857(17) . ?
Mg2 O1 2.1393(16) 2_767 ?
Mg2 O1 2.1393(16) 1_445 ?
O4 Mg3 2.0976(15) 1_655 ?
O1 Mg2 2.1394(15) 1_665 ?
O8 Mg1 2.1156(17) 1_545 ?
N3 C1 1.319(3) . ?
N3 H3C 0.8600 . ?
N3 H3D 0.8600 . ?
N2 C1 1.329(3) . ?
N2 H2C 0.8600 . ?
N2 H2D 0.8600 . ?
N1 C1 1.328(3) . ?
N1 H1C 0.8600 . ?
N1 H1D 0.8600 . ?
O11 P6 1.4967(17) . ?
N5 C2 1.324(3) . ?
N5 H5C 0.8600 . ?
N5 H5D 0.8600 . ?
P6 O12 1.5015(16) . ?
P6 H6A 1.34(4) . ?
P6 H6B 1.27(4) . ?
N6 C2 1.324(3) . ?
N6 H6C 0.8600 . ?
N6 H6D 0.8600 . ?
N4 C2 1.327(3) . ?
N4 H4C 0.8600 . ?
N4 H4D 0.8600 . ?
O12 Mg1 2.0921(16) 2_666 ?
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 163.52(11) . . . 1_655 ?
O2 P1 O1 Mg2 -155.74(12) . . . 1_665 ?
O1 P1 O2 Mg1 158.58(11) . . . . ?
O7 P4 O8 Mg1 159.39(13) . . . 1_545 ?
O4 P2 O3 Mg1 -156.38(11) . . . . ?
O8 P4 O7 Mg2 -177.12(13) . . . . ?
O10 P5 O9 Mg1 -106.5(3) . . . . ?
O6 P3 O5 Mg1 106.5(2) . . . . ?
O9 P5 O10 Mg3 -129.2(2) . . . . ?
O5 P3 O6 Mg2 125.9(3) . . . . ?
Mg3 O11 P6 O12 -179.75(13) . . . . ?
O11 P6 O12 Mg1 167.84(12) . . . 2_666 ?
