Redetermination of the crystal structure of catena-poly[aqua-(1,10-phenanthroline-κ2 N,N′)-(μ2-tetraoxidomolybdato(VI)-κ2 O:O′)manganese(II) monohydrate, C12H12N2O6MoMn
Wu-Hua, Chen; Ji, Zhou; Yu-Fan, Wang; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 865–866; doi:10.1515/ncrs-2020-0065

data_8105312
_publ_section_title
;
 Redetermination of the crystal structure of
 catena-poly[aqua-(1,10-phenanthroline-\k2
 N,N&#x2032;)-(\m2-tetraoxidomolybdato(VI)-\k2 O:O&#x2032;)manganese(II)
 monohydrate, C12H12N2O6MoMn
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              865
_journal_page_last               866
_journal_paper_doi               10.1515/ncrs-2020-0065
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C12 H10 Mn Mo N2 O5, H2 O'
_chemical_formula_sum            'C12 H12 Mn Mo N2 O6'
_chemical_formula_weight         431.12
_chemical_name_common
;
catena-tris(2-oxo)-1'10-phenanthroline-hydrate-molybdenum(vi)-
manganese(ii) solvate hydrate
;
_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
_cell_angle_alpha                73.233(6)
_cell_angle_beta                 83.372(4)
_cell_angle_gamma                77.340(4)
_cell_formula_units_Z            2
_cell_length_a                   7.0427(3)
_cell_length_b                   10.4459(7)
_cell_length_c                   10.5778(6)
_cell_measurement_reflns_used    3263
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.5360
_cell_measurement_theta_min      3.9900
_cell_volume                     725.85(7)
_computing_cell_refinement
'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)[1]'
_computing_data_collection
'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)[1]'
_computing_data_reduction
'CrysAlisPro 1.171.38.41k (Rigaku OD, 2015)[1]'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)[2]'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)[2]'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)[3]'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)[4]'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1151
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.845
_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    -34.00  44.00   1.00    4.53    --  -17.52  57.00 -90.00   78
  2  \w     56.00  83.00   1.00    4.53    --   15.88  77.00 -60.00   27
  3  \w     -1.00  83.00   1.00    4.53    --   15.88  57.00-180.00   84
  4  \w     -4.00  32.00   1.00    4.53    --   15.88  77.00 -60.00   36
  5  \w     -3.00  43.00   1.00    4.53    --   15.88 -77.00  60.00   46
  6  \w     37.00  65.00   1.00    4.53    --   15.88-118.00 -48.00   28
  7  \w    -44.00  32.00   1.00    4.53    --   15.88 -77.00  30.00   76
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Xcalibur, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0012768000
_diffrn_orient_matrix_UB_12      0.0093857000
_diffrn_orient_matrix_UB_13      -0.0690579000
_diffrn_orient_matrix_UB_21      0.0598966000
_diffrn_orient_matrix_UB_22      -0.0654321000
_diffrn_orient_matrix_UB_23      0.0064621000
_diffrn_orient_matrix_UB_31      -0.0842573000
_diffrn_orient_matrix_UB_32      -0.0293172000
_diffrn_orient_matrix_UB_33      0.0104500000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.845
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6071
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.845
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.219
_diffrn_reflns_theta_min         3.263
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.763
_exptl_absorpt_correction_T_max  0.809
_exptl_absorpt_correction_T_min  0.760
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41k (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'translucent light yellow'
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_description       irregular
_exptl_crystal_F_000             426
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.326
_refine_diff_density_min         -1.478
_refine_diff_density_rms         0.124
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         3334
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.177
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0386
_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^)+(0.0400P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0882
_refine_ls_wR_factor_ref         0.0916
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2954
_reflns_number_total             3334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0065_suppl.cif
_cod_data_source_block           zj0415-q5
_cod_database_code               8105312
_chemical_oxdiff_formula         'C H N O Mo Mn Co Ni'
_reflns_odcompleteness_completeness 99.73
_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) groups, All O(H,H) groups
2. Restrained distances
 O5-H5B
 0.82 with sigma of 0.002
 O6-H6A
 0.82 with sigma of 0.002
3. Uiso/Uaniso restraints and constraints
Mo1 \\sim O1 \\sim O2 \\sim O3 \\sim O4: within 2A with sigma of 0.005 and
sigma for terminal atoms of 0.01
O4 \\sim Mn1 \\sim Mo1: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
4.a Free rotating group:
 O6(H6A,H6B)
4.b Rotating group:
 O5(H5A)
4.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C1(H1), C8(H8), C2(H2), C3(H3), C9(H9), C5(H5), C6(H6)
;