[Am]Mn(H2POO)3: A New Family of Hybrid Perovskites Based on the Hypophosphite Ligand.
Wu, Yue; Shaker, Sammy; Brivio, Federico; Murugavel, Ramaswamy; Bristowe, Paul D.; Cheetham, Anthony K.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b09417

data_4126751
_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
;
  1 omega  -36.00  -10.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -      -27.2013   37.0000  -60.0000 26

  2 omega  -49.00   25.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -      -27.2013   37.0000 -180.0000 74

  3 omega   62.00   88.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -       26.2638  178.0000 -120.0000 26

  4 omega -107.00   25.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -      -27.2013  -37.0000 -150.0000 132

  5 omega -104.00  -34.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -      -27.2013  -57.0000    0.0000 70

  6 omega -118.00  -36.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -      -27.2013 -178.0000  -30.0000 82

  7 omega   75.00  113.00   1.0000    3.7050
omega____ theta____ kappa____ phi______ frames
    -       26.2638  178.0000   60.0000 38

  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       '\w 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/[\s^2^(Fo^2^)+(0.0576P)^2^+0.4174P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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_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'