#------------------------------------------------------------------------------
#$Date: 2020-08-08 01:18:08 +0300 (Sat, 08 Aug 2020) $
#$Revision: 255185 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/00/36/4003655.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_4003655
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                105.6072(9)
_cell_angle_beta                 91.0437(9)
_cell_angle_gamma                118.4883(11)
_cell_formula_units_Z            2
_cell_length_a                   8.99858(10)
_cell_length_b                   9.06439(9)
_cell_length_c                   15.67955(16)
_cell_measurement_reflns_used    9386
_cell_measurement_temperature    340(2)
_cell_measurement_theta_max      73.6360
_cell_measurement_theta_min      5.6620
_cell_volume                     1066.28(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      340(2)
_diffrn_measured_fraction_theta_full 0.994
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0294
_diffrn_reflns_Laue_measured_fraction_full 0.994
_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            10557
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.836
_diffrn_reflns_theta_min         5.666
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.886
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59949
_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    1.740
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_refine_diff_density_max         1.233
_refine_diff_density_min         -0.690
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0148(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   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     305
_refine_ls_number_reflns         4168
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0464
_refine_ls_R_factor_gt           0.0461
_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)+(0.0617P)²+2.0027P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1194
_refine_ls_wR_factor_ref         0.1197
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4143
_reflns_number_total             4168
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            exp_38_10_340_00.cif
_cod_data_source_block           exp_38_10_340_00
_cod_database_code               4003655
_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 0.87598(9) 0.71812(9) 0.15534(5) 0.02392(19) Uani 1 1 d . . . . .
P3 P 0.47072(10) 0.70752(11) 0.35573(6) 0.0338(2) Uani 1 1 d . . . . .
P5 P 0.33058(9) 0.85867(10) 0.15705(6) 0.0327(2) Uani 1 1 d . . . . .
Mg3 Mg 0.0000 0.5000 0.0000 0.0146(2) Uani 1 2 d S . P . .
Mg1 Mg 0.73963(10) 0.98470(10) 0.25109(5) 0.0149(2) Uani 1 1 d . . . . .
Mg2 Mg 0.5000 0.5000 0.5000 0.0159(3) Uani 1 2 d S . P . .
O4 O 0.8349(2) 0.5615(2) 0.07512(13) 0.0238(4) Uani 1 1 d . . . . .
O3 O 0.7289(2) 0.7481(2) 0.17783(13) 0.0261(4) Uani 1 1 d . . . . .
O9 O 0.5146(3) 0.9117(3) 0.17186(16) 0.0377(5) Uani 1 1 d . . . . .
O5 O 0.6097(3) 0.8718(3) 0.34331(15) 0.0365(5) Uani 1 1 d . . . . .
O10 O 0.2060(3) 0.6752(3) 0.10237(16) 0.0422(6) Uani 1 1 d . . . . .
O6 O 0.5177(4) 0.6187(4) 0.4051(2) 0.0659(9) Uani 1 1 d . . . . .
P4 P 0.61522(9) 0.25948(10) 0.35583(5) 0.0303(2) Uani 1 1 d . . . . .
O8 O 0.7568(2) 0.2213(2) 0.33367(13) 0.0261(4) Uani 1 1 d . . . . .
O7 O 0.6599(3) 0.4145(3) 0.43646(18) 0.0463(7) Uani 1 1 d . . . . .
P1 P 1.15166(8) 1.22436(9) 0.33708(5) 0.02247(19) Uani 1 1 d . . . . .
O2 O 0.9797(2) 1.0605(2) 0.32159(13) 0.0239(4) Uani 1 1 d . . . . .
O1 O 1.2793(2) 1.2663(3) 0.41541(13) 0.0273(4) Uani 1 1 d . . . . .
N5 N 0.3795(4) 0.4463(4) 0.10504(19) 0.0384(6) Uani 1 1 d . . . . .
H5C H 0.2951 0.4591 0.1225 0.046 Uiso 1 1 calc R U . . .
H5D H 0.4833 0.5306 0.1267 0.046 Uiso 1 1 calc R U . . .
N4 N 0.4780(4) 0.2725(4) 0.0202(2) 0.0399(7) Uani 1 1 d . . . . .
H4C H 0.5823 0.3541 0.0433 0.048 Uiso 1 1 calc R U . . .
H4D H 0.4571 0.1750 -0.0189 0.048 Uiso 1 1 calc R U . . .
C2 C 0.3497(4) 0.2973(4) 0.04501(19) 0.0258(6) Uani 1 1 d . . . . .
N6 N 0.1896(3) 0.1686(3) 0.01222(18) 0.0313(6) Uani 1 1 d . . . . .
H6C H 0.1058 0.1824 0.0300 0.038 Uiso 1 1 calc R U . . .
H6D H 0.1691 0.0712 -0.0269 0.038 Uiso 1 1 calc R U . . .
N3 N 0.9159(4) 0.7741(4) 0.39585(18) 0.0371(6) Uani 1 1 d . . . . .
H3C H 0.9315 0.8510 0.3695 0.044 Uiso 1 1 calc R U . . .
H3D H 0.8181 0.6785 0.3842 0.044 Uiso 1 1 calc R U . . .
C1 C 1.0412(4) 0.8027(4) 0.45385(18) 0.0247(6) Uani 1 1 d . . . . .
N2 N 1.0183(3) 0.6797(3) 0.49132(17) 0.0306(5) Uani 1 1 d . . . . .
H2C H 0.9219 0.5821 0.4775 0.037 Uiso 1 1 calc R U . . .
H2D H 1.1000 0.6977 0.5294 0.037 Uiso 1 1 calc R U . . .
N1 N 1.1925(4) 0.9489(4) 0.4727(2) 0.0397(6) Uani 1 1 d . . . . .
H1C H 1.2099 1.0269 0.4469 0.048 Uiso 1 1 calc R U . . .
H1D H 1.2735 0.9659 0.5109 0.048 Uiso 1 1 calc R U . . .
O11 O 0.0423(3) 0.6938(3) -0.05990(15) 0.0356(5) Uani 1 1 d . . . . .
P6 P 0.11647(10) 0.72865(10) -0.14139(5) 0.0287(2) Uani 1 1 d . . . . .
O12 O 0.1329(3) 0.8893(3) -0.15932(13) 0.0267(4) Uani 1 1 d . . . . .
H2A H 0.944(5) 0.710(5) 0.221(2) 0.031(9) Uiso 1 1 d . . . . .
H2B H 1.010(4) 0.863(5) 0.145(2) 0.032(9) Uiso 1 1 d . . . . .
H5A H 0.309(7) 0.967(7) 0.119(3) 0.075(15) Uiso 1 1 d . . . . .
H1A H 1.132(5) 1.363(5) 0.349(2) 0.037(10) Uiso 1 1 d . . . . .
H1B H 1.224(4) 1.217(5) 0.269(2) 0.029(8) Uiso 1 1 d . . . . .
H6A H 0.016(6) 0.576(7) -0.211(3) 0.071(15) Uiso 1 1 d . . . . .
H4A H 0.478(5) 0.123(5) 0.362(3) 0.046(11) Uiso 1 1 d . . . . .
H3A H 0.345(8) 0.743(8) 0.399(4) 0.11(2) Uiso 1 1 d . . . . .
H4B H 0.552(6) 0.282(6) 0.289(3) 0.055(12) Uiso 1 1 d . . . . .
H3B H 0.371(6) 0.598(7) 0.280(3) 0.070(14) Uiso 1 1 d . . . . .
H6B H 0.266(7) 0.748(7) -0.138(4) 0.084(17) Uiso 1 1 d . . . . .
H5B H 0.278(6) 0.881(6) 0.236(3) 0.059(13) 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 109.9(17) . . ?
O3 P2 H2A 110.2(17) . . ?
O4 P2 H2B 108.6(15) . . ?
O3 P2 H2B 111.7(15) . . ?
H2A P2 H2B 99(2) . . ?
O6 P3 O5 118.13(16) . . ?
O6 P3 H3A 107(3) . . ?
O5 P3 H3A 110(3) . . ?
O6 P3 H3B 111(2) . . ?
O5 P3 H3B 111(2) . . ?
H3A P3 H3B 98(3) . . ?
O10 P5 O9 118.39(14) . . ?
O10 P5 H5A 107(2) . . ?
O9 P5 H5A 110(2) . . ?
O10 P5 H5B 105(2) . . ?
O9 P5 H5B 110(2) . . ?
H5A P5 H5B 106(3) . . ?
O10 Mg3 O10 180.0 . 2_565 ?
O10 Mg3 O11 87.46(10) . 2_565 ?
O10 Mg3 O11 92.54(10) 2_565 2_565 ?
O10 Mg3 O11 92.54(10) . . ?
O10 Mg3 O11 87.46(10) 2_565 . ?
O11 Mg3 O11 180.0 2_565 . ?
O10 Mg3 O4 91.14(9) . 1_455 ?
O10 Mg3 O4 88.86(9) 2_565 1_455 ?
O11 Mg3 O4 90.04(8) 2_565 1_455 ?
O11 Mg3 O4 89.96(8) . 1_455 ?
O10 Mg3 O4 88.86(9) . 2_665 ?
O10 Mg3 O4 91.14(9) 2_565 2_665 ?
O11 Mg3 O4 89.96(8) 2_565 2_665 ?
O11 Mg3 O4 90.04(8) . 2_665 ?
O4 Mg3 O4 180.00(9) 1_455 2_665 ?
O5 Mg1 O9 92.26(10) . . ?
O5 Mg1 O12 176.60(9) . 2_675 ?
O9 Mg1 O12 86.39(10) . 2_675 ?
O5 Mg1 O3 91.34(9) . . ?
O9 Mg1 O3 90.36(9) . . ?
O12 Mg1 O3 91.79(8) 2_675 . ?
O5 Mg1 O2 92.49(9) . . ?
O9 Mg1 O2 174.86(9) . . ?
O12 Mg1 O2 88.98(8) 2_675 . ?
O3 Mg1 O2 87.56(8) . . ?
O5 Mg1 O8 85.86(9) . 1_565 ?
O9 Mg1 O8 92.91(9) . 1_565 ?
O12 Mg1 O8 91.10(8) 2_675 1_565 ?
O3 Mg1 O8 175.77(9) . 1_565 ?
O2 Mg1 O8 89.40(8) . 1_565 ?
O6 Mg2 O6 180.0 2_666 . ?
O6 Mg2 O7 92.96(14) 2_666 . ?
O6 Mg2 O7 87.04(14) . . ?
O6 Mg2 O7 87.04(14) 2_666 2_666 ?
O6 Mg2 O7 92.96(14) . 2_666 ?
O7 Mg2 O7 180.0 . 2_666 ?
O6 Mg2 O1 89.43(10) 2_666 2_776 ?
O6 Mg2 O1 90.57(10) . 2_776 ?
O7 Mg2 O1 89.74(8) . 2_776 ?
O7 Mg2 O1 90.26(8) 2_666 2_776 ?
O6 Mg2 O1 90.57(10) 2_666 1_445 ?
O6 Mg2 O1 89.43(10) . 1_445 ?
O7 Mg2 O1 90.26(8) . 1_445 ?
O7 Mg2 O1 89.74(8) 2_666 1_445 ?
O1 Mg2 O1 180.0 2_776 1_445 ?
P2 O4 Mg3 129.84(12) . 1_655 ?
P2 O3 Mg1 128.01(12) . . ?
P5 O9 Mg1 152.92(17) . . ?
P3 O5 Mg1 144.86(15) . . ?
P5 O10 Mg3 149.85(18) . . ?
P3 O6 Mg2 155.0(3) . . ?
O7 P4 O8 116.04(12) . . ?
O7 P4 H4A 109.1(18) . . ?
O8 P4 H4A 112.7(18) . . ?
O7 P4 H4B 108(2) . . ?
O8 P4 H4B 111(2) . . ?
H4A P4 H4B 99(3) . . ?
P4 O8 Mg1 128.73(12) . 1_545 ?
P4 O7 Mg2 129.28(13) . . ?
O1 P1 O2 116.03(11) . . ?
O1 P1 H1A 107.4(16) . . ?
O2 P1 H1A 110.0(16) . . ?
O1 P1 H1B 106.1(16) . . ?
O2 P1 H1B 111.4(16) . . ?
H1A P1 H1B 105(2) . . ?
P1 O2 Mg1 130.67(12) . . ?
P1 O1 Mg2 135.44(12) . 1_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 . . ?
N5 C2 N6 119.4(3) . . ?
N5 C2 N4 120.8(3) . . ?
N6 C2 N4 119.7(3) . . ?
C2 N6 H6C 120.0 . . ?
C2 N6 H6D 120.0 . . ?
H6C N6 H6D 120.0 . . ?
C1 N3 H3C 120.0 . . ?
C1 N3 H3D 120.0 . . ?
H3C N3 H3D 120.0 . . ?
N3 C1 N1 121.0(3) . . ?
N3 C1 N2 119.6(3) . . ?
N1 C1 N2 119.4(3) . . ?
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 . . ?
P6 O11 Mg3 132.19(12) . . ?
O11 P6 O12 115.56(11) . . ?
O11 P6 H6A 105(2) . . ?
O12 P6 H6A 113(2) . . ?
O11 P6 H6B 112(2) . . ?
O12 P6 H6B 105(3) . . ?
H6A P6 H6B 105(3) . . ?
P6 O12 Mg1 130.15(12) . 2_675 ?
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 1.5017(19) . ?
P2 O3 1.5023(19) . ?
P2 H2A 1.22(4) . ?
P2 H2B 1.35(4) . ?
P3 O6 1.441(3) . ?
P3 O5 1.486(2) . ?
P3 H3A 1.45(7) . ?
P3 H3B 1.30(5) . ?
P5 O10 1.475(2) . ?
P5 O9 1.481(2) . ?
P5 H5A 1.36(5) . ?
P5 H5B 1.33(5) . ?
Mg3 O10 2.061(2) . ?
Mg3 O10 2.061(2) 2_565 ?
Mg3 O11 2.0922(19) 2_565 ?
Mg3 O11 2.0922(19) . ?
Mg3 O4 2.0991(18) 1_455 ?
Mg3 O4 2.0991(18) 2_665 ?
Mg1 O5 2.055(2) . ?
Mg1 O9 2.066(2) . ?
Mg1 O12 2.094(2) 2_675 ?
Mg1 O3 2.0982(19) . ?
Mg1 O2 2.109(2) . ?
Mg1 O8 2.117(2) 1_565 ?
Mg2 O6 2.025(2) 2_666 ?
Mg2 O6 2.025(2) . ?
Mg2 O7 2.089(2) . ?
Mg2 O7 2.089(2) 2_666 ?
Mg2 O1 2.1378(19) 2_776 ?
Mg2 O1 2.1378(19) 1_445 ?
O4 Mg3 2.0991(18) 1_655 ?
P4 O7 1.490(2) . ?
P4 O8 1.4956(19) . ?
P4 H4A 1.30(4) . ?
P4 H4B 1.29(4) . ?
O8 Mg1 2.117(2) 1_545 ?
P1 O1 1.501(2) . ?
P1 O2 1.5033(19) . ?
P1 H1A 1.32(4) . ?
P1 H1B 1.26(3) . ?
O1 Mg2 2.1378(19) 1_665 ?
N5 C2 1.321(4) . ?
N5 H5C 0.8600 . ?
N5 H5D 0.8600 . ?
N4 C2 1.323(4) . ?
N4 H4C 0.8600 . ?
N4 H4D 0.8600 . ?
C2 N6 1.322(4) . ?
N6 H6C 0.8600 . ?
N6 H6D 0.8600 . ?
N3 C1 1.312(4) . ?
N3 H3C 0.8600 . ?
N3 H3D 0.8600 . ?
C1 N1 1.323(4) . ?
C1 N2 1.330(4) . ?
N2 H2C 0.8600 . ?
N2 H2D 0.8600 . ?
N1 H1C 0.8600 . ?
N1 H1D 0.8600 . ?
O11 P6 1.492(2) . ?
P6 O12 1.4961(19) . ?
P6 H6A 1.37(5) . ?
P6 H6B 1.27(6) . ?
O12 Mg1 2.094(2) 2_675 ?
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 163.81(13) . . . 1_655 ?
O4 P2 O3 Mg1 -157.15(14) . . . . ?
O10 P5 O9 Mg1 -110.1(3) . . . . ?
O6 P3 O5 Mg1 113.4(3) . . . . ?
O9 P5 O10 Mg3 -132.4(3) . . . . ?
O5 P3 O6 Mg2 131.0(4) . . . . ?
O7 P4 O8 Mg1 161.66(17) . . . 1_545 ?
O8 P4 O7 Mg2 -172.72(18) . . . . ?
O1 P1 O2 Mg1 159.03(14) . . . . ?
O2 P1 O1 Mg2 -156.10(15) . . . 1_665 ?
Mg3 O11 P6 O12 -176.98(17) . . . . ?
O11 P6 O12 Mg1 169.58(16) . . . 2_675 ?
