#------------------------------------------------------------------------------
#$Date: 2022-03-25 12:12:31 +0200 (Fri, 25 Mar 2022) $
#$Revision: 273993 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/48/8104878.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_8104878
loop_
_publ_author_name
'Jie, Yin'
'Feng-Jun, Zhang'
'Xi-Shi, Tai'
_publ_section_title
;
 The crystal structure of trans-tetraaqua-bis(4-acetylphenoxyacetato-κ1
 O)manganese(II), C20H26O12Mn
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              45
_journal_page_last               46
_journal_paper_doi               10.1515/ncrs-2020-0467
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         'C20 H26 Mn O12'
_chemical_formula_sum            'C20 H26 Mn O12'
_chemical_formula_weight         513.35
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 95.312(13)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.8272(7)
_cell_length_b                   15.828(2)
_cell_length_c                   14.3688(19)
_cell_measurement_reflns_used    1741
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      29.3040
_cell_measurement_theta_min      4.7020
_cell_volume                     1093.1(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -55.00  35.00   1.00    2.50    --   11.90 -57.00 120.00   90
  2  ω    -54.00  36.00   1.00    2.50    --   11.90 -57.00   0.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0762703000
_diffrn_orient_matrix_UB_12      0.0226143000
_diffrn_orient_matrix_UB_13      -0.0317786000
_diffrn_orient_matrix_UB_21      -0.0723744000
_diffrn_orient_matrix_UB_22      -0.0219001000
_diffrn_orient_matrix_UB_23      -0.0378304000
_diffrn_orient_matrix_UB_31      -0.1037150000
_diffrn_orient_matrix_UB_32      0.0319021000
_diffrn_orient_matrix_UB_33      -0.0034511000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4474
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.574
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.669
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90144
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       block
_exptl_crystal_F_000             534
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.281
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         1925
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0413
_refine_ls_R_factor_gt           0.0344
_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/[σ²(Fo²)+(0.0273P)²+0.6334P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0789
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1674
_reflns_number_total             1925
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_j_ncrs-2020-0467_suppl.cif
_cod_data_source_block           04
_cod_database_code               8104878
_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.
;
_reflns_odcompleteness_completeness 99.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Rotating group:
 O5(H5A,H5B), O6(H6A,H6B)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C8(H8), C7(H7)
2.d Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 1.000000 0.500000 1.000000 0.01095(15) Uani 1 2 d S . P . .
O5 O 1.2743(3) 0.44508(9) 0.90025(10) 0.0144(3) Uani 1 1 d . . . . .
H5A H 1.391173 0.482161 0.885822 0.022 Uiso 1 1 d R U . . .
H5B H 1.178751 0.433991 0.848788 0.022 Uiso 1 1 d R U . . .
O6 O 1.2228(3) 0.61997(9) 0.99972(10) 0.0152(3) Uani 1 1 d . . . . .
H6A H 1.201280 0.641493 0.945269 0.023 Uiso 1 1 d R U . . .
H6B H 1.396747 0.610820 1.009177 0.023 Uiso 1 1 d R U . . .
O1 O 0.7213(3) 0.54470(9) 0.88328(10) 0.0149(3) Uani 1 1 d . . . . .
O3 O 0.6974(3) 0.64515(9) 0.66092(10) 0.0163(3) Uani 1 1 d . . . . .
O2 O 0.9950(3) 0.64264(10) 0.82568(10) 0.0201(4) Uani 1 1 d . . . . .
O4 O -0.0238(3) 0.59254(10) 0.27330(11) 0.0238(4) Uani 1 1 d . . . . .
C1 C 0.7932(4) 0.59373(13) 0.81885(14) 0.0130(5) Uani 1 1 d . . . . .
C2 C 0.6044(4) 0.58808(13) 0.72874(14) 0.0148(5) Uani 1 1 d . . . . .
H2A H 0.605262 0.530793 0.704778 0.018 Uiso 1 1 calc R U . . .
H2B H 0.415273 0.602071 0.740719 0.018 Uiso 1 1 calc R U . . .
C3 C 0.5562(4) 0.64356(13) 0.57383(14) 0.0142(5) Uani 1 1 d . . . . .
C6 C 0.3074(4) 0.64485(13) 0.38965(15) 0.0141(5) Uani 1 1 d . . . . .
C4 C 0.6551(5) 0.69783(14) 0.50818(15) 0.0184(5) Uani 1 1 d . . . . .
H4 H 0.803584 0.733719 0.525428 0.022 Uiso 1 1 calc R U . . .
C9 C 0.1719(5) 0.64214(13) 0.29306(15) 0.0172(5) Uani 1 1 d . . . . .
C5 C 0.5326(5) 0.69830(13) 0.41744(15) 0.0173(5) Uani 1 1 d . . . . .
H5 H 0.600264 0.734606 0.373964 0.021 Uiso 1 1 calc R U . . .
C10 C 0.2683(5) 0.69943(14) 0.22004(15) 0.0188(5) Uani 1 1 d . . . . .
H10A H 0.196595 0.679850 0.159299 0.028 Uiso 1 1 calc R U . . .
H10B H 0.467918 0.699569 0.224255 0.028 Uiso 1 1 calc R U . . .
H10C H 0.202274 0.755688 0.229624 0.028 Uiso 1 1 calc R U . . .
C8 C 0.3308(5) 0.59130(15) 0.54837(16) 0.0241(5) Uani 1 1 d . . . . .
H8 H 0.261152 0.555855 0.592271 0.029 Uiso 1 1 calc R U . . .
C7 C 0.2108(5) 0.59241(15) 0.45711(16) 0.0243(6) Uani 1 1 d . . . . .
H7 H 0.060837 0.556926 0.440411 0.029 Uiso 1 1 calc R U . . .
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'
O O 0.0106 0.0060 '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
O5 Mn1 O5 180.00(7) 3_767 .
O6 Mn1 O5 89.08(5) . 3_767
O6 Mn1 O5 90.92(5) 3_767 3_767
O6 Mn1 O5 90.92(5) . .
O6 Mn1 O5 89.08(5) 3_767 .
O6 Mn1 O6 180.0 . 3_767
O1 Mn1 O5 89.59(5) 3_767 3_767
O1 Mn1 O5 90.41(5) 3_767 .
O1 Mn1 O5 89.59(5) . .
O1 Mn1 O5 90.41(5) . 3_767
O1 Mn1 O6 90.85(5) . 3_767
O1 Mn1 O6 90.85(5) 3_767 .
O1 Mn1 O6 89.15(5) . .
O1 Mn1 O6 89.15(5) 3_767 3_767
O1 Mn1 O1 180.00(7) 3_767 .
Mn1 O5 H5A 109.6 . .
Mn1 O5 H5B 109.5 . .
H5A O5 H5B 104.3 . .
Mn1 O6 H6A 109.4 . .
Mn1 O6 H6B 109.3 . .
H6A O6 H6B 104.5 . .
C1 O1 Mn1 124.51(13) . .
C3 O3 C2 116.74(16) . .
O1 C1 C2 113.59(18) . .
O2 C1 O1 125.75(19) . .
O2 C1 C2 120.66(18) . .
O3 C2 C1 110.04(17) . .
O3 C2 H2A 109.7 . .
O3 C2 H2B 109.7 . .
C1 C2 H2A 109.7 . .
C1 C2 H2B 109.7 . .
H2A C2 H2B 108.2 . .
O3 C3 C4 115.79(19) . .
O3 C3 C8 124.30(19) . .
C8 C3 C4 119.9(2) . .
C5 C6 C9 123.16(19) . .
C7 C6 C9 119.3(2) . .
C7 C6 C5 117.5(2) . .
C3 C4 H4 120.0 . .
C5 C4 C3 119.9(2) . .
C5 C4 H4 120.0 . .
O4 C9 C6 119.6(2) . .
O4 C9 C10 120.2(2) . .
C6 C9 C10 120.2(2) . .
C6 C5 H5 119.4 . .
C4 C5 C6 121.1(2) . .
C4 C5 H5 119.4 . .
C9 C10 H10A 109.5 . .
C9 C10 H10B 109.5 . .
C9 C10 H10C 109.5 . .
H10A C10 H10B 109.5 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C3 C8 H8 120.3 . .
C3 C8 C7 119.4(2) . .
C7 C8 H8 120.3 . .
C6 C7 C8 122.1(2) . .
C6 C7 H7 119.0 . .
C8 C7 H7 119.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O5 2.2169(14) .
Mn1 O5 2.2169(14) 3_767
Mn1 O6 2.1825(14) .
Mn1 O6 2.1825(14) 3_767
Mn1 O1 2.1692(14) .
Mn1 O1 2.1692(14) 3_767
O5 H5A 0.8527 .
O5 H5B 0.8528 .
O6 H6A 0.8508 .
O6 H6B 0.8507 .
O1 C1 1.280(2) .
O3 C2 1.431(2) .
O3 C3 1.369(2) .
O2 C1 1.241(3) .
O4 C9 1.241(3) .
C1 C2 1.516(3) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C3 C4 1.393(3) .
C3 C8 1.388(3) .
C6 C9 1.479(3) .
C6 C5 1.406(3) .
C6 C7 1.389(3) .
C4 H4 0.9300 .
C4 C5 1.381(3) .
C9 C10 1.493(3) .
C5 H5 0.9300 .
C10 H10A 0.9600 .
C10 H10B 0.9600 .
C10 H10C 0.9600 .
C8 H8 0.9300 .
C8 C7 1.384(3) .
C7 H7 0.9300 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
Mn1 O1 C1 O2 -23.2(3) . . . .
Mn1 O1 C1 C2 157.07(13) . . . .
O1 C1 C2 O3 179.51(16) . . . .
O3 C3 C4 C5 177.54(19) . . . .
O3 C3 C8 C7 -177.3(2) . . . .
O2 C1 C2 O3 -0.3(3) . . . .
C2 O3 C3 C4 -178.21(18) . . . .
C2 O3 C3 C8 0.6(3) . . . .
C3 O3 C2 C1 176.32(16) . . . .
C3 C4 C5 C6 0.2(3) . . . .
C3 C8 C7 C6 -0.5(4) . . . .
C4 C3 C8 C7 1.5(3) . . . .
C9 C6 C5 C4 -179.1(2) . . . .
C9 C6 C7 C8 179.2(2) . . . .
C5 C6 C9 O4 179.1(2) . . . .
C5 C6 C9 C10 -1.6(3) . . . .
C5 C6 C7 C8 -0.6(3) . . . .
C8 C3 C4 C5 -1.3(3) . . . .
C7 C6 C9 O4 -0.8(3) . . . .
C7 C6 C9 C10 178.6(2) . . . .
C7 C6 C5 C4 0.8(3) . . . .
