The crystal structure of diaqua-bis(pyrazolo[1,5-a]pyrimidine-3-carboxylato-κ2 N,O)manganese(II), C14H12N6O6Mn
Hong, Dong-Feng; Li, Meng-Fei; Chu, Tian-Tian; Zeitschrift für Kristallographie - New Crystal Structures 237 (2022) 613–614; doi:10.1515/ncrs-2022-0143

data_8107168
_publ_section_title
;
 The crystal structure of
 diaqua-bis(pyrazolo[1,5-a]pyrimidine-3-carboxylato-\k2 N,O)manganese(II),
 C14H12N6O6Mn
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              613
_journal_page_last               614
_journal_paper_doi               10.1515/ncrs-2022-0143
_journal_volume                  237
_journal_year                    2022
_chemical_formula_moiety         'C14 H12 Mn N6 O6'
_chemical_formula_sum            'C14 H12 Mn N6 O6'
_chemical_formula_weight         415.24
_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                 112.359(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.0839(3)
_cell_length_b                   13.1211(4)
_cell_length_c                   8.9854(3)
_cell_measurement_reflns_used    5490
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.0780
_cell_measurement_theta_min      3.9300
_cell_volume                     772.39(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.121a (Rigaku OD, 2021)'
_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_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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     -1.00  84.00   1.00   10.00    --   17.09  38.00-180.00   85
  2  \w    -15.00  56.00   1.00   10.00    --   17.09 -99.00   0.00   71
  3  \w    -48.00  34.00   1.00   10.00    --   17.09 -57.00-120.00   82
  4  \w    -36.00  32.00   1.00   10.00    --   17.09 -38.00  60.00   68
  5  \w     -7.00  42.00   1.00   10.00    --   17.09  77.00 -30.00   49
  6  \w     10.00  81.00   1.00   10.00    --   17.09  57.00-120.00   71
  7  \w    -10.00  41.00   1.00   10.00    --   17.09  77.00 120.00   51
  8  \w    -15.00  11.00   1.00   10.00    --   17.09 -99.00  60.00   26
  9  \w     25.00  56.00   1.00   10.00    --   17.09 -99.00  60.00   31
 10  \w     -7.00  43.00   1.00   10.00    --   17.09  19.00  60.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0868383000
_diffrn_orient_matrix_UB_12      0.0169000000
_diffrn_orient_matrix_UB_13      -0.0141952000
_diffrn_orient_matrix_UB_21      0.0541355000
_diffrn_orient_matrix_UB_22      -0.0442013000
_diffrn_orient_matrix_UB_23      0.0387346000
_diffrn_orient_matrix_UB_31      -0.0355057000
_diffrn_orient_matrix_UB_32      -0.0261151000
_diffrn_orient_matrix_UB_33      -0.0747002000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            8374
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        24.982
_diffrn_reflns_theta_max         24.982
_diffrn_reflns_theta_min         3.476
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.121a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       block
_exptl_crystal_F_000             422
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.31
_refine_diff_density_max         0.244
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.047
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     125
_refine_ls_number_reflns         1352
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0311P)^2^+0.5130P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0711
_refine_ls_wR_factor_ref         0.0725
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1269
_reflns_number_total             1352
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0143_suppl.cif
_cod_data_source_block           mnn_auto
_cod_original_cell_volume        772.39(5)
_cod_database_code               8107168
_shelx_estimated_absorpt_t_max   0.766
_shelx_estimated_absorpt_t_min   0.742
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2.a Rotating group:
 O3(H3A,H3B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C6(H6), C7(H7)
;
_shelx_res_checksum              39577
_shelx_hkl_checksum              62603
_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 1.226
_oxdiff_exptl_absorpt_empirical_full_min 0.803