#------------------------------------------------------------------------------
#$Date: 2022-11-08 11:28:34 +0200 (Tue, 08 Nov 2022) $
#$Revision: 279087 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/60/8106008.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_8106008
loop_
_publ_author_name
'Zhang, Tian'
_publ_section_title
;
 Crystal structure of
 poly[diaqua-bis(μ2-3-((1H-imidazol-1-yl)methyl)benzoato-κ2N:O)manganese(II)],
 C22H22MnN4O6
;
_journal_issue                   6
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              1285
_journal_page_last               1286
_journal_paper_doi               10.1515/ncrs-2019-0411
_journal_volume                  234
_journal_year                    2019
_chemical_formula_moiety         '0.5(C44 H44 Mn2 N8 O12)'
_chemical_formula_sum            'C22 H22 Mn N4 O6'
_chemical_formula_weight         493.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 107.391(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.9331(7)
_cell_length_b                   5.5962(3)
_cell_length_c                   16.0671(9)
_cell_measurement_reflns_used    2844
_cell_measurement_temperature    286.74(11)
_cell_measurement_theta_max      27.3020
_cell_measurement_theta_min      4.0860
_cell_volume                     1023.91(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)[1]'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)[1]'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)[1]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)[4]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[4]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)[3]'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)[2]'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      286.74(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -80.00   4.00   1.00    5.00    --  -12.53 -57.00-150.00   84
  2  ω    -85.00 -35.00   1.00    5.00    --  -12.53-178.00 -60.00   50
  3  ω    -56.00  32.00   1.00    5.00    --   13.55 -38.00 120.00   88
  4  ω     34.00  86.00   1.00    5.00    --   13.55-178.00   0.00   52
  5  ω    -80.00 -55.00   1.00    5.00    --  -12.53 -77.00  90.00   25
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0506185000
_diffrn_orient_matrix_UB_12      -0.0735866000
_diffrn_orient_matrix_UB_13      0.0134221000
_diffrn_orient_matrix_UB_21      0.0197743000
_diffrn_orient_matrix_UB_22      0.0650345000
_diffrn_orient_matrix_UB_23      0.0395931000
_diffrn_orient_matrix_UB_31      -0.0304103000
_diffrn_orient_matrix_UB_32      -0.0801121000
_diffrn_orient_matrix_UB_33      0.0198182000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            5738
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.491
_diffrn_reflns_theta_min         3.578
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.695
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68907
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41r (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    1.600
_exptl_crystal_description       block
_exptl_crystal_F_000             510
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.524
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     151
_refine_ls_number_reflns         1882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.136
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0461
_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)+(0.0370P)²+1.6540P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1653
_reflns_number_total             1882
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2019-0411_suppl.cif
_cod_data_source_block           2
_cod_original_cell_volume        1023.92(11)
_cod_database_code               8106008
_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 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.66
_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 O(H,H) groups
2.a Riding coordinates:
 O1(H1A,H1B)
2.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C7(H7), C9(H9), C10(H10), C11(H11)
;
_olex2_date_sample_data_collection 2017-05-11
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.590
_oxdiff_exptl_absorpt_empirical_full_min 0.731
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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 0.5000 1.0000 0.5000 0.0168(2) Uani 1 2 d S T P . .
O1 O 0.3663(2) 0.7120(4) 0.46752(16) 0.0376(6) Uani 1 1 d . . . . .
H1A H 0.3919 0.5881 0.4979 0.056 Uiso 1 1 d R . . . .
H1B H 0.3063 0.7826 0.4738 0.056 Uiso 1 1 d R . . . .
O2 O 0.6255(2) 0.7630(4) 0.46449(17) 0.0373(6) Uani 1 1 d . . . . .
O3 O 0.7902(2) 0.9809(4) 0.50252(18) 0.0423(7) Uani 1 1 d . . . . .
N1 N 1.0637(3) 0.6210(6) 0.14321(18) 0.0349(7) Uani 1 1 d . . . . .
N2 N 1.0832(2) 0.6085(5) 0.28382(18) 0.0305(7) Uani 1 1 d . . . . .
C1 C 0.7302(3) 0.8105(6) 0.4635(2) 0.0288(8) Uani 1 1 d . . . . .
C2 C 0.7828(3) 0.6403(6) 0.4122(2) 0.0269(7) Uani 1 1 d . . . . .
C3 C 0.7157(3) 0.4515(6) 0.3664(2) 0.0313(8) Uani 1 1 d . . . . .
H3 H 0.6436 0.4393 0.3635 0.038 Uiso 1 1 calc R . . . .
C4 C 0.7673(3) 0.2833(6) 0.3257(2) 0.0347(8) Uani 1 1 d . . . . .
H4 H 0.7267 0.1677 0.2980 0.042 Uiso 1 1 calc R . . . .
C5 C 0.8827(3) 0.3034(6) 0.3300(2) 0.0324(8) Uani 1 1 d . . . . .
H5 H 0.9144 0.1950 0.3075 0.039 Uiso 1 1 calc R . . . .
C6 C 0.9491(3) 0.4971(6) 0.3702(2) 0.0287(8) Uani 1 1 d . . . . .
C7 C 0.8988(3) 0.6636(6) 0.4120(2) 0.0277(7) Uani 1 1 d . . . . .
H7 H 0.9394 0.7816 0.4379 0.033 Uiso 1 1 calc R . . . .
C8 C 1.0749(3) 0.5223(7) 0.3687(2) 0.0345(9) Uani 1 1 d . . . . .
H8A H 1.1108 0.6194 0.4084 0.041 Uiso 1 1 calc R . . . .
H8B H 1.1089 0.3875 0.3800 0.041 Uiso 1 1 calc R . . . .
C9 C 1.1331(4) 0.8175(7) 0.2687(2) 0.0432(10) Uani 1 1 d . . . . .
H9 H 1.1653 0.9234 0.3061 0.052 Uiso 1 1 calc R . . . .
C10 C 1.1210(4) 0.8223(8) 0.1826(2) 0.0449(10) Uani 1 1 d . . . . .
H10 H 1.1454 0.9339 0.1565 0.054 Uiso 1 1 calc R . . . .
C11 C 1.0442(4) 0.4976(7) 0.2065(2) 0.0384(9) Uani 1 1 d . . . . .
H11 H 1.0106 0.3620 0.1995 0.046 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'
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
O1 Mn1 O1 180.0 . 3_676
O1 Mn1 N1 88.80(10) 3_676 4_576
O1 Mn1 N1 88.80(10) . 2_655
O1 Mn1 N1 91.20(10) . 4_576
O1 Mn1 N1 91.20(10) 3_676 2_655
O2 Mn1 O1 89.91(9) 3_676 3_676
O2 Mn1 O1 90.09(9) . 3_676
O2 Mn1 O1 89.91(9) . .
O2 Mn1 O1 90.09(9) 3_676 .
O2 Mn1 O2 180.0 3_676 .
O2 Mn1 N1 88.01(10) . 2_655
O2 Mn1 N1 88.01(10) 3_676 4_576
O2 Mn1 N1 91.99(10) . 4_576
O2 Mn1 N1 91.99(10) 3_676 2_655
N1 Mn1 N1 180.0 4_576 2_655
Mn1 O1 H1A 110.3 . .
Mn1 O1 H1B 101.9 . .
H1A O1 H1B 118.9 . .
C1 O2 Mn1 128.3(2) . .
C10 N1 Mn1 132.4(2) . 2_645
C11 N1 Mn1 122.7(3) . 2_645
C11 N1 C10 104.8(3) . .
C9 N2 C8 126.6(3) . .
C11 N2 C8 127.1(3) . .
C11 N2 C9 106.3(3) . .
O2 C1 C2 116.2(3) . .
O3 C1 O2 124.7(3) . .
O3 C1 C2 119.1(3) . .
C3 C2 C1 119.8(3) . .
C7 C2 C1 121.1(3) . .
C7 C2 C3 119.0(3) . .
C2 C3 H3 120.1 . .
C4 C3 C2 119.7(3) . .
C4 C3 H3 120.1 . .
C3 C4 H4 119.9 . .
C5 C4 C3 120.2(3) . .
C5 C4 H4 119.9 . .
C4 C5 H5 119.4 . .
C4 C5 C6 121.1(3) . .
C6 C5 H5 119.4 . .
C5 C6 C7 118.9(3) . .
C5 C6 C8 119.8(3) . .
C7 C6 C8 121.3(3) . .
C2 C7 H7 119.6 . .
C6 C7 C2 120.9(3) . .
C6 C7 H7 119.6 . .
N2 C8 C6 112.6(3) . .
N2 C8 H8A 109.1 . .
N2 C8 H8B 109.1 . .
C6 C8 H8A 109.1 . .
C6 C8 H8B 109.1 . .
H8A C8 H8B 107.8 . .
N2 C9 H9 126.8 . .
C10 C9 N2 106.3(4) . .
C10 C9 H9 126.8 . .
N1 C10 H10 125.0 . .
C9 C10 N1 110.1(4) . .
C9 C10 H10 125.0 . .
N1 C11 N2 112.5(3) . .
N1 C11 H11 123.7 . .
N2 C11 H11 123.7 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Mn1 O1 2.218(2) .
Mn1 O1 2.218(2) 3_676
Mn1 O2 2.200(2) 3_676
Mn1 O2 2.200(2) .
Mn1 N1 2.299(3) 2_655
Mn1 N1 2.299(3) 4_576
O1 H1A 0.8501 .
O1 H1B 0.8502 .
O2 C1 1.281(4) .
O3 C1 1.244(4) .
N1 Mn1 2.299(3) 2_645
N1 C10 1.370(5) .
N1 C11 1.307(5) .
N2 C8 1.478(4) .
N2 C9 1.367(5) .
N2 C11 1.341(5) .
C1 C2 1.514(5) .
C2 C3 1.395(5) .
C2 C7 1.391(5) .
C3 H3 0.8500 .
C3 C4 1.391(5) .
C4 H4 0.8500 .
C4 C5 1.363(5) .
C5 H5 0.8500 .
C5 C6 1.384(5) .
C6 C7 1.386(5) .
C6 C8 1.515(5) .
C7 H7 0.8500 .
C8 H8A 0.8500 .
C8 H8B 0.8500 .
C9 H9 0.8500 .
C9 C10 1.348(5) .
C10 H10 0.8500 .
C11 H11 0.8500 .
