#------------------------------------------------------------------------------
#$Date: 2017-11-21 02:08:19 +0200 (Tue, 21 Nov 2017) $
#$Revision: 203363 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/67/4126751.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_4126751
loop_
_publ_author_name
'Wu, Yue'
'Shaker, Sammy'
'Brivio, Federico'
'Murugavel, Ramaswamy'
'Bristowe, Paul D.'
'Cheetham, Anthony K.'
_publ_section_title
;
 [Am]Mn(H2POO)3: A New Family of Hybrid Perovskites Based on the
 Hypophosphite Ligand.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b09417
_journal_year                    2017
_chemical_formula_moiety         'H12 Mn2 O12 P6, 2(C H6 N3)'
_chemical_formula_sum            'C2 H24 Mn2 N6 O12 P6'
_chemical_formula_weight         619.97
_chemical_name_systematic        'Guanidinium manganese hypophosphite'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-08-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                105.294(6)
_cell_angle_beta                 90.971(6)
_cell_angle_gamma                118.618(8)
_cell_formula_units_Z            2
_cell_length_a                   9.0994(7)
_cell_length_b                   9.2419(6)
_cell_length_c                   15.8369(12)
_cell_measurement_reflns_used    3875
_cell_measurement_temperature    302(1)
_cell_measurement_theta_max      28.0980
_cell_measurement_theta_min      2.5470
_cell_volume                     1111.44(18)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      302(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1183
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.882
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -36.00  -10.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -      -27.2013   37.0000  -60.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega  -49.00   25.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -      -27.2013   37.0000 -180.0000 74

#__ type_ start__ end____ width___ exp.time_
  3 omega   62.00   88.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -       26.2638  178.0000 -120.0000 26

#__ type_ start__ end____ width___ exp.time_
  4 omega -107.00   25.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -      -27.2013  -37.0000 -150.0000 132

#__ type_ start__ end____ width___ exp.time_
  5 omega -104.00  -34.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -      -27.2013  -57.0000    0.0000 70

#__ type_ start__ end____ width___ exp.time_
  6 omega -118.00  -36.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -      -27.2013 -178.0000  -30.0000 82

#__ type_ start__ end____ width___ exp.time_
  7 omega   75.00  113.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -       26.2638  178.0000   60.0000 38

#__ type_ start__ end____ width___ exp.time_
  8 omega   58.00  118.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -       26.2638  178.0000  -60.0000 60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0743664000
_diffrn_orient_matrix_UB_12      -0.0376788000
_diffrn_orient_matrix_UB_13      0.0187613000
_diffrn_orient_matrix_UB_21      0.0507485000
_diffrn_orient_matrix_UB_22      0.0319542000
_diffrn_orient_matrix_UB_23      0.0422656000
_diffrn_orient_matrix_UB_31      -0.0034903000
_diffrn_orient_matrix_UB_32      0.0775536000
_diffrn_orient_matrix_UB_33      0.0090039000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_av_unetI/netI     0.0574
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.882
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8592
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.882
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.299
_diffrn_reflns_theta_min         2.567
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.628
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.93873
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_description       irregular
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.277
_refine_diff_density_min         -0.881
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         4879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_gt           0.0468
_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)+(0.0576P)²+0.4174P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1250
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4175
_reflns_number_total             4879
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja7b09417_si_005.cif
_cod_data_source_block           ywsms-mnhypogua-dmso3
_cod_original_cell_volume        1111.44(16)
_cod_database_code               4126751
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Mn H12 P3 O6 N3 C'
_chemical_oxdiff_usercomment
'Full sphere for beta phase of GUA-Mn-H2PO2 perovskite (P-1)'
_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.
;
_shelx_estimated_absorpt_t_max   0.737
_shelx_estimated_absorpt_t_min   0.659
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups, All P(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 P5(H5a,H5b), P8(H8a,H8b), P11(H11a,H11b), P14(H14a,H14b), P17(H17a,H17b),
 P20(H20a,H20b)
2.b X=CH2 refined with riding coordinates:
 N25(H25a,H25b), N22(H22a,H22b), N29(H29a,H29b), N26(H26a,H26b), N24(H24a,
 H24b), N28(H28a,H28b)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
Mn1 Mn 0.26476(5) 0.02110(5) 0.24849(3) 0.01604(13) Uani 1 1 d . . .
Mn2 Mn 0.000000 0.500000 0.500000 0.01565(16) Uani 1 2 d S T P
Mn3 Mn -0.500000 -0.500000 0.000000 0.01703(16) Uani 1 2 d S T P
P5 P -0.15195(10) -0.21038(10) 0.16427(6) 0.0225(2) Uani 1 1 d . . .
H5A H -0.125495 -0.350660 0.155010 0.027 Uiso 1 1 calc R . .
H5B H -0.223844 -0.190332 0.240909 0.027 Uiso 1 1 calc R . .
P8 P 0.13862(11) 0.30008(11) 0.34109(6) 0.0246(2) Uani 1 1 d . . .
H8A H 0.006303 0.149220 0.352584 0.029 Uiso 1 1 calc R . .
H8B H 0.079023 0.327354 0.268030 0.029 Uiso 1 1 calc R . .
P11 P -0.46002(12) -0.70228(11) 0.14512(6) 0.0300(2) Uani 1 1 d . . .
H11A H -0.371349 -0.593726 0.230559 0.036 Uiso 1 1 calc R . .
H11B H -0.343488 -0.727577 0.095728 0.036 Uiso 1 1 calc R . .
P14 P 0.11713(13) 0.73853(11) 0.36196(6) 0.0292(2) Uani 1 1 d . . .
H14A H 0.014967 0.591467 0.289462 0.035 Uiso 1 1 calc R . .
H14B H 0.280163 0.759371 0.369176 0.035 Uiso 1 1 calc R . .
P17 P 0.67369(11) 0.14330(12) 0.34185(7) 0.0304(2) Uani 1 1 d . . .
H17A H 0.711036 0.104995 0.256154 0.036 Uiso 1 1 calc R . .
H17B H 0.705817 0.045294 0.385466 0.036 Uiso 1 1 calc R . .
P20 P -0.62422(12) -0.26574(12) 0.14280(7) 0.0324(2) Uani 1 1 d . . .
H20A H -0.484599 -0.117370 0.133511 0.039 Uiso 1 1 calc R . .
H20B H -0.573253 -0.301838 0.214862 0.039 Uiso 1 1 calc R . .
O4 O -0.2776(3) -0.2547(3) 0.08573(16) 0.0281(5) Uani 1 1 d . . .
O7 O 0.2829(3) 0.2691(3) 0.31918(16) 0.0269(5) Uani 1 1 d . . .
O19 O -0.6688(3) -0.4137(3) 0.0609(2) 0.0430(7) Uani 1 1 d . . .
O9 O 0.1781(3) 0.4497(3) 0.42209(15) 0.0240(5) Uani 1 1 d . . .
O21 O -0.7624(3) -0.2254(3) 0.16457(16) 0.0265(5) Uani 1 1 d . . .
O6 O 0.0178(3) -0.0497(3) 0.17772(16) 0.0249(5) Uani 1 1 d . . .
O13 O 0.1273(3) 0.8934(3) 0.34309(16) 0.0261(5) Uani 1 1 d . . .
O10 O -0.5899(4) -0.8733(3) 0.15258(17) 0.0358(6) Uani 1 1 d . . .
O15 O 0.0482(3) 0.7069(3) 0.44381(17) 0.0333(6) Uani 1 1 d . . .
O16 O 0.4889(3) 0.0825(3) 0.33337(18) 0.0366(6) Uani 1 1 d . . .
O18 O 0.7950(3) 0.3301(3) 0.38917(18) 0.0384(7) Uani 1 1 d . . .
N25 N -0.1854(3) -0.1698(3) 0.4942(2) 0.0283(6) Uani 1 1 d . . .
H25A H -0.102064 -0.184000 0.478371 0.034 Uiso 1 1 calc R . .
H25B H -0.165962 -0.075347 0.533302 0.034 Uiso 1 1 calc R . .
O12 O -0.5200(4) -0.6104(4) 0.1048(2) 0.0570(9) Uani 1 1 d . . .
N22 N -0.3733(4) -0.4384(4) 0.3985(2) 0.0354(7) Uani 1 1 d . . .
H22A H -0.290015 -0.452636 0.382643 0.042 Uiso 1 1 calc R . .
H22B H -0.476088 -0.518680 0.375315 0.042 Uiso 1 1 calc R . .
N29 N -0.0182(4) 0.3156(3) 0.0042(2) 0.0288(7) Uani 1 1 d . . .
H29A H -0.099561 0.301035 -0.031697 0.035 Uiso 1 1 calc R . .
H29B H 0.079333 0.408434 0.015877 0.035 Uiso 1 1 calc R . .
N26 N 0.0807(4) 0.2229(4) 0.1001(2) 0.0334(7) Uani 1 1 d . . .
H26A H 0.176090 0.318634 0.113464 0.040 Uiso 1 1 calc R . .
H26B H 0.065770 0.145373 0.124640 0.040 Uiso 1 1 calc R . .
N24 N -0.4719(4) -0.2696(4) 0.4824(2) 0.0336(7) Uani 1 1 d . . .
H24A H -0.574732 -0.348872 0.458766 0.040 Uiso 1 1 calc R . .
H24B H -0.451977 -0.174940 0.521516 0.040 Uiso 1 1 calc R . .
C23 C -0.3435(4) -0.2933(4) 0.4585(2) 0.0237(7) Uani 1 1 d . . .
N28 N -0.1931(4) 0.0520(4) 0.0236(2) 0.0341(7) Uani 1 1 d . . .
H28A H -0.274533 0.037364 -0.012272 0.041 Uiso 1 1 calc R . .
H28B H -0.209101 -0.026206 0.047895 0.041 Uiso 1 1 calc R . .
C27 C -0.0431(4) 0.1950(4) 0.0415(2) 0.0247(7) Uani 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 0.0033 0.0016 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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
O7 Mn1 O21 174.02(9) . 1_655
O7 Mn1 O6 86.33(9) . .
O6 Mn1 O21 89.44(9) . 1_655
O13 Mn1 O7 93.65(9) 1_545 .
O13 Mn1 O21 90.40(9) 1_545 1_655
O13 Mn1 O6 87.81(9) 1_545 .
O10 Mn1 O7 92.01(9) 1_665 .
O10 Mn1 O21 84.19(9) 1_665 1_655
O10 Mn1 O6 95.45(10) 1_665 .
O10 Mn1 O13 173.65(9) 1_665 1_545
O10 Mn1 O16 92.46(11) 1_665 .
O16 Mn1 O7 91.97(9) . .
O16 Mn1 O21 92.80(9) . 1_655
O16 Mn1 O6 171.96(10) . .
O16 Mn1 O13 84.46(10) . 1_545
O9 Mn2 O9 180.00(12) . 2_566
O15 Mn2 O9 89.05(9) . .
O15 Mn2 O9 90.94(9) 2_566 .
O15 Mn2 O9 89.05(9) 2_566 2_566
O15 Mn2 O9 90.95(9) . 2_566
O15 Mn2 O15 180.0 . 2_566
O18 Mn2 O9 89.52(10) 1_455 2_566
O18 Mn2 O9 89.52(10) 2_666 .
O18 Mn2 O9 90.48(10) 2_666 2_566
O18 Mn2 O9 90.48(10) 1_455 .
O18 Mn2 O15 93.42(11) 1_455 2_566
O18 Mn2 O15 86.58(11) 1_455 .
O18 Mn2 O15 93.42(11) 2_666 .
O18 Mn2 O15 86.58(11) 2_666 2_566
O18 Mn2 O18 180.0 2_666 1_455
O4 Mn3 O4 180.0 2_445 .
O19 Mn3 O4 90.51(9) . 2_445
O19 Mn3 O4 90.51(9) 2_445 .
O19 Mn3 O4 89.49(9) . .
O19 Mn3 O4 89.49(9) 2_445 2_445
O19 Mn3 O19 180.0 2_445 .
O12 Mn3 O4 90.96(11) . 2_445
O12 Mn3 O4 90.96(11) 2_445 .
O12 Mn3 O4 89.04(11) . .
O12 Mn3 O4 89.04(11) 2_445 2_445
O12 Mn3 O19 94.22(13) . 2_445
O12 Mn3 O19 85.78(13) 2_445 2_445
O12 Mn3 O19 94.22(13) 2_445 .
O12 Mn3 O19 85.78(13) . .
O12 Mn3 O12 180.0 . 2_445
O4 P5 O6 115.60(14) . .
O7 P8 O9 116.13(13) . .
O12 P11 O10 117.54(19) . .
O15 P14 O13 114.89(14) . .
O16 P17 O18 118.08(16) . .
O19 P20 O21 115.79(14) . .
P5 O4 Mn3 134.20(14) . .
P8 O7 Mn1 126.92(13) . .
P20 O19 Mn3 127.39(15) . .
P8 O9 Mn2 128.42(14) . .
P20 O21 Mn1 127.63(13) . 1_455
P5 O6 Mn1 129.01(13) . .
P14 O13 Mn1 127.82(14) . 1_565
P11 O10 Mn1 139.25(16) . 1_445
P14 O15 Mn2 130.22(14) . .
P17 O16 Mn1 145.80(19) . .
P17 O18 Mn2 142.34(18) . 1_655
P11 O12 Mn3 144.6(2) . .
N25 C23 N24 119.7(3) . .
N22 C23 N25 120.0(3) . .
N22 C23 N24 120.3(3) . .
N29 C27 N26 119.3(3) . .
N29 C27 N28 120.1(3) . .
N28 C27 N26 120.5(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O7 2.193(2) .
Mn1 O21 2.206(2) 1_655
Mn1 O6 2.203(2) .
Mn1 O13 2.187(2) 1_545
Mn1 O10 2.150(3) 1_665
Mn1 O16 2.164(2) .
Mn2 O9 2.203(2) 2_566
Mn2 O9 2.203(2) .
Mn2 O15 2.179(2) .
Mn2 O15 2.179(2) 2_566
Mn2 O18 2.158(2) 1_455
Mn2 O18 2.158(2) 2_666
Mn3 O4 2.228(2) 2_445
Mn3 O4 2.228(2) .
Mn3 O19 2.178(3) 2_445
Mn3 O19 2.178(3) .
Mn3 O12 2.135(3) 2_445
Mn3 O12 2.134(3) .
P5 O4 1.502(2) .
P5 O6 1.504(2) .
P8 O7 1.500(2) .
P8 O9 1.503(2) .
P11 O10 1.491(2) .
P11 O12 1.464(3) .
P14 O13 1.499(2) .
P14 O15 1.487(3) .
P17 O16 1.486(3) .
P17 O18 1.491(3) .
P20 O19 1.494(3) .
P20 O21 1.495(2) .
N25 C23 1.323(4) .
N22 C23 1.322(4) .
N29 C27 1.323(4) .
N26 C27 1.325(4) .
N24 C23 1.332(4) .
N28 C27 1.323(4) .
