Crystal structure of poly[diaqua-bis(μ2-3-((1H-imidazol-1-yl)methyl)benzoato-κ2N:O)manganese(II)], C22H22MnN4O6
Zhang, Tian; Zeitschrift für Kristallographie - New Crystal Structures 234 (2019) 1285–1286; doi:10.1515/ncrs-2019-0411

data_8106008
_publ_section_title
;
 Crystal structure of
 poly[diaqua-bis(\m2-3-((1H-imidazol-1-yl)methyl)benzoato-\k2N:O)manganese(II)],
 C22H22MnN4O6
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur 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  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -80.00   4.00   1.00    5.00    --  -12.53 -57.00-150.00   84
  2  \w    -85.00 -35.00   1.00    5.00    --  -12.53-178.00 -60.00   50
  3  \w    -56.00  32.00   1.00    5.00    --   13.55 -38.00 120.00   88
  4  \w     34.00  86.00   1.00    5.00    --   13.55-178.00   0.00   52
  5  \w    -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       '\w 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/[\s^2^(Fo^2^)+(0.0370P)^2^+1.6540P] where P=(Fo^2^+2Fc^2^)/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 > 2\s(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
_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)
;
_shelx_res_checksum              31178
_shelx_hkl_checksum              9614
_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