[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_4126747
_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         '0.08(H48 Mn8 O48 P24), 0.33(C6 H14 N2)'
_chemical_formula_sum            'C2 H8.67 Mn0.67 N0.67 O4 P2'
_chemical_formula_weight         204.66
_chemical_name_systematic        'Dabconium 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     dual
_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                66.631(7)
_cell_angle_beta                 89.585(4)
_cell_angle_gamma                89.082(6)
_cell_formula_units_Z            12
_cell_length_a                   9.8364(6)
_cell_length_b                   14.9329(13)
_cell_length_c                   16.8019(9)
_cell_measurement_reflns_used    5901
_cell_measurement_temperature    120.2(8)
_cell_measurement_theta_max      27.9270
_cell_measurement_theta_min      2.4370
_cell_volume                     2265.2(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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      120.2(8)
_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 0.878
_diffrn_measurement_details
;
  1 omega   62.00  118.00   1.0000   25.7400
omega____ theta____ kappa____ phi______ frames
    -       26.2638  178.0000  120.0000 56

  2 omega   64.00   95.00   1.0000   25.7400
omega____ theta____ kappa____ phi______ frames
    -       26.2638  178.0000 -180.0000 31

  3 omega -119.00  -74.00   1.0000   25.7400
omega____ theta____ kappa____ phi______ frames
    -      -27.2013 -178.0000   60.0000 45

  4 omega  -10.00   19.00   1.0000   25.7400
omega____ theta____ kappa____ phi______ frames
    -      -27.2013   37.0000 -120.0000 29

  5 omega  -45.00   -2.00   1.0000   25.7400
omega____ theta____ kappa____ phi______ frames
    -      -27.2013   37.0000  -60.0000 43

  6 omega  -38.00   54.00   1.0000   25.7400
omega____ theta____ kappa____ phi______ frames
    -      -27.2013   37.0000 -180.0000 92

  7 omega  -49.00   54.00   1.0000   25.7400
omega____ theta____ kappa____ phi______ frames
    -      -27.2013   37.0000   90.0000 103

  8 omega   17.00   43.00   1.0000   25.7400
omega____ theta____ kappa____ phi______ frames
    -      -27.2013   37.0000  -60.0000 26

  9 omega  -55.00   31.00   1.0000   25.7400
omega____ theta____ kappa____ phi______ frames
    -      -27.2013   77.0000  -60.0000 86
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0042124000
_diffrn_orient_matrix_UB_12      0.0471394000
_diffrn_orient_matrix_UB_13      -0.0337981000
_diffrn_orient_matrix_UB_21      0.0430292000
_diffrn_orient_matrix_UB_22      -0.0189874000
_diffrn_orient_matrix_UB_23      -0.0238020000
_diffrn_orient_matrix_UB_31      -0.0577234000
_diffrn_orient_matrix_UB_32      -0.0098036000
_diffrn_orient_matrix_UB_33      -0.0201517000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0349
_diffrn_reflns_av_unetI/netI     0.0549
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17271
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.878
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.303
_diffrn_reflns_theta_min         1.486
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.592
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69898
_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    1.800
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1248
_exptl_crystal_size_max          0.346
_exptl_crystal_size_mid          0.223
_exptl_crystal_size_min          0.176
_refine_diff_density_max         2.161
_refine_diff_density_min         -1.146
_refine_diff_density_rms         0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.157
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     511
_refine_ls_number_reflns         9898
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.157
_refine_ls_R_factor_all          0.1255
_refine_ls_R_factor_gt           0.1149
_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^)+(0.0500P)^2^+73.0880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2718
_refine_ls_wR_factor_ref         0.2775
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8478
_reflns_number_total             9898
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09417_si_007.cif
_cod_data_source_block           ywsms-mnhypodabco_120k_1_120_00
_cod_database_code               4126747
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Mn P2 O4 C3 N'
_shelx_estimated_absorpt_t_max   0.767
_shelx_estimated_absorpt_t_min   0.609
_reflns_odcompleteness_completeness 87.84
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.24
_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:
 N011(H011), N012(H012), N016(H016), N018(H018)
2.b Secondary CH2 refined with riding coordinates:
 P007(H00A,H00B), P008(H00C,H00D), P009(H00E,H00F), P00A(H00G,H00H), P00B(H00I,
 H00J), P00C(H00K,H00L), P00D(H00M,H00N), P00E(H00O,H00P), P00F(H00Q,H00R),
 P00G(H00S,H00T), P00H(H00U,H00V), P00I(H00W,H00X), C01B(H01A,H01B), C01C(H01C,
 H01D), C01D(H01M,H01N), C01E(H01E,H01F), C01F(H01O,H01P), C01G(H01Q,H01R),
 C01H(H01G,H01H), C01I(H01I,H01J), C01J(H01S,H01T), C01K(H01U,H01V), C01L(H01K,
 H01L), C01M(H01W,H01X)
;
_olex2_submission_special_instructions 'No special instructions were received'