Hydrothemal synthesis and crystal structure of triaqua-bis(5-carboxy-1-methyl-1H-imidazole-4-carboxylato-κ2 N,O;κ1O)manganese(II), C12H16N4O11Mn
Guang-Zhen, Liu; Meng-Zhen, Yan; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 835–836; doi:10.1515/ncrs-2018-0043

data_8106316
_publ_section_title
;
 Hydrothemal synthesis and crystal structure of
 triaqua-bis(5-carboxy-1-methyl-1H-imidazole-4-carboxylato-\k2
 N,O;\k1O)manganese(II), C12H16N4O11Mn
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              835
_journal_page_last               836
_journal_paper_doi               10.1515/ncrs-2018-0043
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C12 H16 Mn N4 O11'
_chemical_formula_sum            'C12 H16 Mn N4 O11'
_chemical_formula_weight         447.23
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                104.288(3)
_cell_angle_beta                 94.024(3)
_cell_angle_gamma                97.365(3)
_cell_formula_units_Z            2
_cell_length_a                   7.7186(3)
_cell_length_b                   9.8439(3)
_cell_length_c                   11.6084(3)
_cell_measurement_reflns_used    8635
_cell_measurement_temperature    291.03(10)
_cell_measurement_theta_max      26.4510
_cell_measurement_theta_min      4.2350
_cell_volume                     842.91(5)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41r (Rigaku OD, 2015)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_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    -20.00  29.00   1.00    3.00    --   -9.62 -99.00-150.00   49
  2  \w    -79.00   9.00   1.00    3.00    --   -9.62 -38.00 -90.00   88
  3  \w    -36.00  58.00   1.00    3.00    --   -9.62  77.00  60.00   94
  4  \w    -19.00  82.00   1.00    3.00    --   10.64  19.00-120.00  101
  5  \w    -20.00  50.00   1.00    3.00    --   10.64 -99.00  30.00   70
  6  \w     -6.00  78.00   1.00    3.00    --   10.64  57.00  90.00   84
  7  \w    -20.00  50.00   1.00    3.00    --   10.64 -99.00-150.00   70
  8  \w    -20.00  50.00   1.00    3.00    --   10.64 -99.00 120.00   70
  9  \w     -6.00  78.00   1.00    3.00    --   10.64  57.00  30.00   84
 10  \w    -56.00  34.00   1.00    3.00    --   10.64 -71.00 -91.00   90
 11  \w    -77.00 -29.00   1.00    3.00    --   -9.62 -77.00 150.00   48
;
_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      -0.0082564000
_diffrn_orient_matrix_UB_12      0.0352246000
_diffrn_orient_matrix_UB_13      -0.0460969000
_diffrn_orient_matrix_UB_21      -0.0766007000
_diffrn_orient_matrix_UB_22      0.0246569000
_diffrn_orient_matrix_UB_23      0.0223610000
_diffrn_orient_matrix_UB_31      0.0524147000
_diffrn_orient_matrix_UB_32      0.0617089000
_diffrn_orient_matrix_UB_33      0.0373603000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14394
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.393
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73839
_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    1.762
_exptl_crystal_description       block
_exptl_crystal_F_000             458
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.27
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         2880
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0322
_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/[\s^2^(Fo^2^)+(0.0383P)^2^+0.5684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0822
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2709
_reflns_number_total             2880
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0043_suppl.cif
_cod_data_source_block           lgz
_cod_original_cell_volume        842.93(5)
_cod_database_code               8106316
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     23.21
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Rotating group:
 O1W(H1WA,H1WB), O2W(H2WA,H2WB), O3W(H3WA,H3WB)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8)
2.c Idealised Me refined as rotating group:
 C4(H4A,H4B,H4C), C11(H11A,H11B,H11C)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3), O7(H7)
;
_olex2_date_sample_data_collection 2017-09-20
_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 1.314
_oxdiff_exptl_absorpt_empirical_full_min 0.590
_publcif_funding_html
;
;