[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_4126753
_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         'H3 Mn0.5 O3 P1.5, C0.5 H3 N1.5'
_chemical_formula_sum            'C0.5 H6 Mn0.5 N1.5 O3 P1.5'
_chemical_formula_weight         154.99
_chemical_name_systematic        'Guanidinium manganese hypophosphite'
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-I 2y'
_space_group_name_H-M_alt        'I 1 2/m 1'
_symmetry_space_group_name_Hall  '-I 2y'
_symmetry_space_group_name_H-M   'I 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2017-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_cell_angle_alpha                90
_cell_angle_beta                 89.764(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.7596(3)
_cell_length_b                   13.2087(4)
_cell_length_c                   9.6956(3)
_cell_measurement_reflns_used    1876
_cell_measurement_temperature    298.3(10)
_cell_measurement_theta_max      28.0570
_cell_measurement_theta_min      2.5910
_cell_volume                     1121.80(6)
_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      298.3(10)
_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 0.932
_diffrn_measurement_details
;
  1 omega   76.00  118.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3419  178.0000   90.0000 42

  2 omega   57.00  107.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -       26.3419  178.0000  -30.0000 50

  3 omega -109.00   26.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1232  -37.0000 -120.0000 135

  4 omega  -45.00   50.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1232   37.0000 -180.0000 95

  5 omega -104.00   -6.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1232  -57.0000   30.0000 98

  6 omega -120.00  -82.00   1.0000   75.0000
omega____ theta____ kappa____ phi______ frames
    -      -27.1232 -178.0000   30.0000 38
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0464698000
_diffrn_orient_matrix_UB_12      0.0187198000
_diffrn_orient_matrix_UB_13      0.0540467000
_diffrn_orient_matrix_UB_21      0.0538392000
_diffrn_orient_matrix_UB_22      -0.0390360000
_diffrn_orient_matrix_UB_23      -0.0127995000
_diffrn_orient_matrix_UB_31      0.0386880000
_diffrn_orient_matrix_UB_32      0.0317817000
_diffrn_orient_matrix_UB_33      -0.0476222000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3906
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.934
_diffrn_reflns_theta_min         2.606
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.613
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.95011
_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 light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.835
_exptl_crystal_description       block
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.202
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.099
_refine_diff_density_max         0.533
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1315
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0303
_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^)+(0.0358P)^2^+2.1602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0757
_refine_ls_wR_factor_ref         0.0790
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1178
_reflns_number_total             1315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b09417_si_004.cif
_cod_data_source_block           ywtb-mn_guafa_4-1_50c_2
_cod_original_cell_volume        1121.79(6)
_cod_original_formula_sum        'C0.50 H6 Mn0.50 N1.50 O3 P1.50'
_cod_database_code               4126753
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Mn P3 O6 C N3'
_chemical_oxdiff_usercomment
'Monoclinic GUA crystal from Mn 4GUA:1FA H3PO2 mixture for better statistics'
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.737
_reflns_odcompleteness_completeness 100.00
_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. Others
 Fixed Sof: H4a(0.5) H4b(0.5) H6b(0.5) H6a(0.5) H10a(0.5) H10b(0.5)
3.a Secondary CH2 refined with riding coordinates:
 P2(H2a,H2b), P4(H4a,H4b), P6(H6b,H6a)
3.b X=CH2 refined with riding coordinates:
 N8(H8a,H8b), N10(H10a,H10b)
;
_olex2_exptl_crystal_mounting_method 'Mounted on loop with immersion oil'
_olex2_submission_special_instructions 'No special instructions were received'