[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_4126750
_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         'H6 Mn O6 P3, C2 H4 N3'
_chemical_formula_sum            'C2 H8 Mn N3 O6 P3'
_chemical_formula_weight         317.96
_chemical_name_systematic        'Triazolium managnese hypophosphite'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2017-08-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
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_cell_angle_alpha                90
_cell_angle_beta                 98.554(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.8034(3)
_cell_length_b                   8.5924(2)
_cell_length_c                   13.3120(4)
_cell_measurement_reflns_used    2257
_cell_measurement_temperature    298.8(4)
_cell_measurement_theta_max      28.0650
_cell_measurement_theta_min      2.1050
_cell_volume                     1108.86(5)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.34i (release 04-08-2014 CrysAlis171 .NET)
(compiled Aug  4 2014,14:34:23)
;
_computing_data_reduction
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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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      298.8(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1183
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.887
_diffrn_measurement_details
;
  1 omega  -31.00    0.00   1.0000    7.8200
omega____ theta____ kappa____ phi______ frames
    -       26.2638  116.0000  -49.0000 31

  2 omega  -66.00   46.00   1.0000    7.8200
omega____ theta____ kappa____ phi______ frames
    -      -27.2013   57.0000   90.0000 112

  3 omega  -99.00   24.00   1.0000    7.8200
omega____ theta____ kappa____ phi______ frames
    -      -27.2013  -19.0000  120.0000 123
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0607279000
_diffrn_orient_matrix_UB_12      0.0436467000
_diffrn_orient_matrix_UB_13      0.0029390000
_diffrn_orient_matrix_UB_21      0.0080218000
_diffrn_orient_matrix_UB_22      -0.0133040000
_diffrn_orient_matrix_UB_23      0.0531141000
_diffrn_orient_matrix_UB_31      0.0400381000
_diffrn_orient_matrix_UB_32      0.0688128000
_diffrn_orient_matrix_UB_33      0.0084216000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0244
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.887
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4414
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.887
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.319
_diffrn_reflns_theta_min         2.101
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.635
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98889
_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 colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.905
_exptl_crystal_description       irregular
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.359
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.223
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.0051(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2451
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0370
_refine_ls_R_factor_gt           0.0305
_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/[\s^2^(Fo^2^)+(0.0249P)^2^+0.5669P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0690
_refine_ls_wR_factor_ref         0.0731
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2151
_reflns_number_total             2451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09417_si_008.cif
_cod_data_source_block           ywsms-mntzlhyp_50c_3
_cod_original_cell_volume        1108.87(5)
_cod_database_code               4126750
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Mn P2 O4 C2 N3'
_chemical_oxdiff_usercomment
'Block crystal from Mn-H2PO2-1,2,4-triazole heating at 50 oC overnight'
_shelx_estimated_absorpt_t_max   0.712
_shelx_estimated_absorpt_t_min   0.591
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups, All P(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 P3(H3A,H3B), P6(H6A,H6B), P9(H9A,H9B)
2.b Aromatic/amide H refined with riding coordinates:
 N16(H16), N15(H15), C11(H11), C14(H14)
;
_olex2_submission_special_instructions 'No special instructions were received'