[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_4126754
_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(C3 H5 N2)'
_chemical_formula_sum            'C6 H22 Mn2 N4 O12 P6'
_chemical_formula_weight         637.97
_chemical_name_systematic        'Imidazolium manganese 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     iterative
_audit_creation_date             2017-08-17
_audit_creation_method
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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                 91.5497(17)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6520(2)
_cell_length_b                   12.7066(2)
_cell_length_c                   18.4643(3)
_cell_measurement_reflns_used    3434
_cell_measurement_temperature    300.00(14)
_cell_measurement_theta_max      27.8160
_cell_measurement_theta_min      1.9480
_cell_volume                     2263.71(7)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      300.00(14)
_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 0.896
_diffrn_measurement_details
;
  1 omega -118.00  -33.00   1.0000    7.7050
omega____ theta____ kappa____ phi______ frames
    -      -27.2013  178.0000 -150.0000 85

  2 omega -107.00    9.00   1.0000    7.7050
omega____ theta____ kappa____ phi______ frames
    -      -27.2013  -77.0000   60.0000 116

  3 omega  -20.00   53.00   1.0000    7.7050
omega____ theta____ kappa____ phi______ frames
    -      -27.2013   37.0000 -180.0000 73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0196069000
_diffrn_orient_matrix_UB_12      -0.0405404000
_diffrn_orient_matrix_UB_13      0.0240440000
_diffrn_orient_matrix_UB_21      0.0487953000
_diffrn_orient_matrix_UB_22      -0.0343437000
_diffrn_orient_matrix_UB_23      -0.0156357000
_diffrn_orient_matrix_UB_31      0.0513673000
_diffrn_orient_matrix_UB_32      0.0172185000
_diffrn_orient_matrix_UB_33      0.0255472000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0218
_diffrn_reflns_av_unetI/netI     0.0383
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.896
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9480
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.896
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.303
_diffrn_reflns_theta_min         1.946
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.599
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86235
_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    1.872
_exptl_crystal_description
;
;
_exptl_crystal_F_000             1288
_exptl_crystal_size_max          0.411
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.105
_refine_diff_density_max         0.440
_refine_diff_density_min         -0.659
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         5033
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0518
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0338P)^2^+1.1665P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0801
_refine_ls_wR_factor_ref         0.0879
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3994
_reflns_number_total             5033
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09417_si_006.cif
_cod_data_source_block           ywsms-mnhypim-lvt_5_300_00
_cod_original_cell_volume        2263.72(8)
_cod_database_code               4126754
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.850
_shelx_estimated_absorpt_t_min   0.559
_reflns_odcompleteness_completeness 89.63
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.24
_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:
 P4(H4A,H4B), P7(H7A,H7B), P10(H10A,H10B), P13(H13A,H13B), P16(H16A,H16B),
 P19(H19A,H19B)
2.b Aromatic/amide H refined with riding coordinates:
 N22(H22), N27(H27), N25(H25), N29(H29), C24(H24), C23(H23), C30(H30),
 C21(H21), C28(H28), C26(H26)
;
_olex2_submission_special_instructions 'No special instructions were received'