#------------------------------------------------------------------------------
#$Date: 2017-11-21 02:08:43 +0200 (Tue, 21 Nov 2017) $
#$Revision: 203364 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/12/67/4126752.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4126752
loop_
_publ_author_name
'Wu, Yue'
'Shaker, Sammy'
'Brivio, Federico'
'Murugavel, Ramaswamy'
'Bristowe, Paul D.'
'Cheetham, Anthony K.'
_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
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   59.00   85.25   0.7500   11.3250
omega____ theta____ kappa____ phi______ frames
    -       26.2638  178.0000  -30.0000 35

#__ type_ start__ end____ width___ exp.time_
  2 omega  -95.00  -32.00   0.7500   11.3250
omega____ theta____ kappa____ phi______ frames
    -      -27.2013  178.0000    0.0000 84

#__ type_ start__ end____ width___ exp.time_
  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       'ω 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/[σ²(Fo²)+(0.0404P)²+28.1920P] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Mn1 Mn 0.666667 0.333333 0.08032(2) 0.0220(3) Uani 1 3 d S T P
Mn2 Mn 0.333333 -0.333333 0.166667 0.0203(3) Uani 1 6 d S T P
Mn3 Mn 1.000000 0.000000 0.000000 0.0213(3) Uani 1 6 d S T P
P5 P 0.85333(14) 0.15872(14) 0.05138(3) 0.0357(3) Uani 1 1 d . . .
H5A H 0.902452 0.167745 0.083595 0.043 Uiso 1 1 calc R . .
H5B H 0.721746 0.010793 0.047072 0.043 Uiso 1 1 calc R . .
P8 P 0.5656(3) 0.03232(18) 0.13575(4) 0.0800(7) Uani 1 1 d . . .
H8A H 0.477892 0.077521 0.154898 0.096 Uiso 1 1 calc R . .
H8B H 0.703449 0.074736 0.152885 0.096 Uiso 1 1 calc R . .
O4 O 0.8049(4) 0.2782(4) 0.04663(8) 0.0444(9) Uani 1 1 d . . .
O7 O 0.4781(4) -0.1392(4) 0.13440(8) 0.0459(9) Uani 1 1 d . . .
C12 C 0.4622(7) 0.6447(8) 0.02535(12) 0.0569(16) Uani 1 1 d . . .
H12A H 0.559615 0.720604 0.015241 0.068 Uiso 1 1 calc R . .
H12B H 0.442134 0.541048 0.019700 0.068 Uiso 1 1 calc R . .
N10 N 0.333333 0.666667 0.07384(14) 0.0331(15) Uani 1 3 d S T P
H10 H 0.333329 0.666667 0.097642 0.040 Uiso 1 3 calc RS T P
N13 N 0.333333 0.666667 0.01345(14) 0.0356(16) Uani 1 3 d S T P
H13 H 0.333329 0.666667 -0.010358 0.043 Uiso 1 3 calc RS T P
O6 O 0.9796(4) 0.1708(4) 0.02972(9) 0.0447(9) Uani 1 1 d . . .
O9 O 0.6091(5) 0.1263(5) 0.10735(10) 0.0635(12) Uani 1 1 d . . .
C11 C 0.4747(6) 0.6653(7) 0.06190(12) 0.0443(13) Uani 1 1 d . . .
H11A H 0.481729 0.580140 0.071907 0.053 Uiso 1 1 calc R . .
H11B H 0.567880 0.762579 0.067496 0.053 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O4 Mn1 O4 84.44(14) . 3_665
O4 Mn1 O4 84.44(14) . 2_655
O4 Mn1 O4 84.44(14) 3_665 2_655
O9 Mn1 O4 172.19(15) . 2_655
O9 Mn1 O4 172.19(15) 3_665 .
O9 Mn1 O4 89.55(15) 3_665 3_665
O9 Mn1 O4 89.55(15) 2_655 2_655
O9 Mn1 O4 89.55(15) . .
O9 Mn1 O4 90.04(16) 3_665 2_655
O9 Mn1 O4 90.04(16) 2_655 .
O9 Mn1 O4 172.20(15) 2_655 3_665
O9 Mn1 O4 90.04(16) . 3_665
O9 Mn1 O9 95.44(16) . 3_665
O9 Mn1 O9 95.44(16) . 2_655
O9 Mn1 O9 95.44(16) 2_655 3_665
O7 Mn2 O7 93.28(13) 14 3_655
O7 Mn2 O7 180.0 15_445 3_655
O7 Mn2 O7 93.28(13) 13_545 2_545
O7 Mn2 O7 180.0 13_545 .
O7 Mn2 O7 86.72(13) 13_545 14
O7 Mn2 O7 86.72(13) 15_445 13_545
O7 Mn2 O7 180.0 14 2_545
O7 Mn2 O7 86.72(13) . 2_545
O7 Mn2 O7 93.28(13) 13_545 3_655
O7 Mn2 O7 93.28(13) 14 .
O7 Mn2 O7 86.72(13) . 3_655
O7 Mn2 O7 93.28(13) 15_445 2_545
O7 Mn2 O7 93.28(13) 15_445 .
O7 Mn2 O7 86.72(13) 15_445 14
O7 Mn2 O7 86.72(13) 2_545 3_655
O6 Mn3 O6 180.0(3) 12_545 3_765
O6 Mn3 O6 88.55(14) 12_545 .
O6 Mn3 O6 88.55(14) 3_765 11_665
O6 Mn3 O6 91.45(14) 3_765 2_645
O6 Mn3 O6 88.55(14) 3_765 10_755
O6 Mn3 O6 91.45(14) 12_545 11_665
O6 Mn3 O6 91.45(14) 10_755 11_665
O6 Mn3 O6 180.0(3) 2_645 11_665
O6 Mn3 O6 91.45(14) 3_765 .
O6 Mn3 O6 88.55(14) 10_755 2_645
O6 Mn3 O6 180.0 10_755 .
O6 Mn3 O6 91.45(14) 2_645 .
O6 Mn3 O6 88.55(14) 12_545 2_645
O6 Mn3 O6 91.45(14) 12_545 10_755
O6 Mn3 O6 88.55(14) 11_665 .
O6 P5 O4 116.4(2) . .
O9 P8 O7 122.3(2) . .
P5 O4 Mn1 126.8(2) . .
P8 O7 Mn2 137.9(2) . .
N13 C12 C11 109.2(4) . .
C11 N10 C11 109.6(3) . 3_565
C11 N10 C11 109.6(3) 2_665 .
C11 N10 C11 109.6(3) 2_665 3_565
C12 N13 C12 109.6(3) 2_665 3_565
C12 N13 C12 109.6(3) 2_665 .
C12 N13 C12 109.6(3) 3_565 .
P5 O6 Mn3 132.3(2) . .
P8 O9 Mn1 154.5(3) . .
N10 C11 C12 108.4(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O4 2.199(3) .
Mn1 O4 2.199(3) 3_665
Mn1 O4 2.199(3) 2_655
Mn1 O9 2.142(4) .
Mn1 O9 2.142(4) 2_655
Mn1 O9 2.142(4) 3_665
Mn2 O7 2.179(3) .
Mn2 O7 2.180(3) 15_445
Mn2 O7 2.180(3) 2_545
Mn2 O7 2.180(3) 13_545
Mn2 O7 2.180(3) 14
Mn2 O7 2.179(3) 3_655
Mn3 O6 2.175(3) 12_545
Mn3 O6 2.175(3) 3_765
Mn3 O6 2.175(3) 11_665
Mn3 O6 2.175(3) 10_755
Mn3 O6 2.175(3) 2_645
Mn3 O6 2.175(3) .
P5 O4 1.492(4) .
P5 O6 1.489(3) .
P8 O7 1.469(4) .
P8 O9 1.420(4) .
C12 N13 1.479(6) .
C12 C11 1.515(7) .
N10 C11 1.488(5) .
N10 C11 1.489(5) 3_565
N10 C11 1.489(5) 2_665
