[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_4126752
_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         'H4 Mn0.67 O4 P2, C2 H4.67 N0.67'
_chemical_formula_sum            'C2 H8.67 Mn0.67 N0.67 O4 P2'
_chemical_formula_weight         204.66
_chemical_name_systematic        '[C6N2H14]Mn[H2PO2]3'
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   9.8860(5)
_cell_length_b                   9.8860(5)
_cell_length_c                   41.171(2)
_cell_measurement_reflns_used    1079
_cell_measurement_temperature    300.0(4)
_cell_measurement_theta_max      27.4090
_cell_measurement_theta_min      2.4320
_cell_volume                     3484.7(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.0(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 0.893
_diffrn_measurement_details
;
  1 omega   59.00   85.25   0.7500   11.3250
omega____ theta____ kappa____ phi______ frames
    -       26.2638  178.0000  -30.0000 35

  2 omega  -95.00  -32.00   0.7500   11.3250
omega____ theta____ kappa____ phi______ frames
    -      -27.2013  178.0000    0.0000 84

  3 omega  -48.00   14.25   0.7500   11.3250
omega____ theta____ kappa____ phi______ frames
    -      -27.2013   43.0000   32.0000 83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0752319000
_diffrn_orient_matrix_UB_12      0.0303840000
_diffrn_orient_matrix_UB_13      0.0070419000
_diffrn_orient_matrix_UB_21      0.0056526000
_diffrn_orient_matrix_UB_22      -0.0633726000
_diffrn_orient_matrix_UB_23      -0.0065087000
_diffrn_orient_matrix_UB_31      0.0343132000
_diffrn_orient_matrix_UB_32      0.0437235000
_diffrn_orient_matrix_UB_33      -0.0143195000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0221
_diffrn_reflns_av_unetI/netI     0.0439
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            2742
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.237
_diffrn_reflns_theta_min         2.430
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.552
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84597
_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    1.755
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1872
_exptl_crystal_preparation       'MnCO3, H2PO3 and dabco (C6N2H12) dissolved'
_exptl_crystal_recrystallization_method 'Slow evaporation on hotplate at 50 C'
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.176
_refine_diff_density_max         0.807
_refine_diff_density_min         -1.221
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     86
_refine_ls_number_reflns         1717
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0584
_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^)+(0.0404P)^2^+28.1920P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1248
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1362
_reflns_number_total             1717
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09417_si_009.cif
_cod_data_source_block           ywsms-mnhypodabco-50c_4
_cod_original_cell_volume        3484.7(4)
_cod_database_code               4126752
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Mn H4 P2 O4 N2 C6'
_chemical_oxdiff_usercomment
'Irregular clear shard of Mn H2PO2 DABCO heated 50 oC overnight'
_shelx_estimated_absorpt_t_max   0.772
_shelx_estimated_absorpt_t_min   0.616
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups, All P(H,H) groups
2.a Ternary CH refined with riding coordinates:
 N10(H10), N13(H13)
2.b Secondary CH2 refined with riding coordinates:
 P5(H5A,H5B), P8(H8A,H8B), C12(H12A,H12B), C11(H11A,H11B)
;
_olex2_exptl_crystal_mounting_method 'Mounted on loop with immersion oil'
_olex2_submission_special_instructions 'No special instructions were received'