Hypophosphite hybrid perovskites: a platform for unconventional tilts and shifts.
Wu, Yue; Binford, Trevor; Hill, Joshua A.; Shaker, Sammy; Wang, John; Cheetham, Anthony K.; Chemical communications (Cambridge, England) 54 (2018) 3751–3754; doi:10.1039/c8cc00907d

data_7121457
_publ_section_title
;
 Hypophosphite hybrid perovskites: a platform for unconventional tilts and
 shifts.
;
_journal_issue                   30
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3751
_journal_page_last               3754
_journal_paper_doi               10.1039/c8cc00907d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'H18 Mn3 O18 P9, 3(C2 H8 N)'
_chemical_formula_sum            'C6 H42 Mn3 N3 O18 P9'
_chemical_formula_weight         887.97
_chemical_name_systematic        'Dimethylammonium 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             2018-01-11
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-01-29 deposited with the CCDC.
2018-03-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.188(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.6139(3)
_cell_length_b                   13.3050(3)
_cell_length_c                   19.3418(6)
_cell_measurement_reflns_used    4406
_cell_measurement_temperature    298.9(6)
_cell_measurement_theta_max      28.0310
_cell_measurement_theta_min      1.8910
_cell_volume                     3551.85(17)
_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      298.9(6)
_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  -80.00   10.00   1.0000   14.0850
omega____ theta____ kappa____ phi______ frames
    -      -27.1232  -57.0000 -150.0000 90

  2 omega  -64.00   35.00   1.0000   14.0850
omega____ theta____ kappa____ phi______ frames
    -      -27.1232   57.0000   30.0000 99

  3 omega  -64.00   23.00   1.0000   14.0850
omega____ theta____ kappa____ phi______ frames
    -      -27.1232   57.0000  150.0000 87
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0018050000
_diffrn_orient_matrix_UB_12      0.0126944000
_diffrn_orient_matrix_UB_13      0.0360475000
_diffrn_orient_matrix_UB_21      -0.0459174000
_diffrn_orient_matrix_UB_22      -0.0229033000
_diffrn_orient_matrix_UB_23      -0.0063820000
_diffrn_orient_matrix_UB_31      0.0230766000
_diffrn_orient_matrix_UB_32      -0.0463982000
_diffrn_orient_matrix_UB_33      0.0129686000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0263
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.878
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            14768
_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         28.363
_diffrn_reflns_theta_min         1.475
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.519
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96373
_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    1.661
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.529
_exptl_crystal_size_mid          0.468
_exptl_crystal_size_min          0.352
_refine_diff_density_max         0.788
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.084
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         7802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0455P)^2^+3.4521P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5873
_reflns_number_total             7802
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc00907d2.cif
_cod_data_source_block           yw-mn_tmaoh_hp_dmf_4
_cod_depositor_comments          'Adding full bibliography for 7121457.cif.'
_cod_original_cell_volume        3551.84(17)
_cod_database_code               7121457
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'Mn P2 C2 O6 N3'
_chemical_oxdiff_usercomment
'Roughly cubic large crystal of Mn-TMAOH-HP_DMF stood for several months (likely Mn-DMA-HP)'
_shelx_estimated_absorpt_t_max   0.617
_shelx_estimated_absorpt_t_min   0.500
_reflns_odcompleteness_completeness 99.91
_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
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 P1(H1A,H1B), P2(H2A,H2B), P3(H3A,H3B), P4(H4A,H4B), P5(H5A,H5B), P6(H6A,H6B),
 P7(H7A,H7B), P8(H8A,H8B), P9(H9A,H9B), N(HA,HB), N0AA(H0AA,H0AB), N1(H1C,H1D)
2.b Idealised Me refined as rotating group:
 C1AA(H1AA,H1AB,H1AC), C(HC,HD,HE), C2AA(H2AA,H2AB,H2AC), C3AA(H3AA,H3AB,H3AC),
  C0AA(H0AC,H0AD,H0AE), C15(H15A,H15B,H15C)
;
_olex2_exptl_crystal_mounting_method 'Mounted with paratone oil on cryoloop'
_olex2_submission_special_instructions 'No special instructions were received'