The crystal structure of catena-poly[(1,10-phenanthroline-k2 N,N′)-(μ3-tetraoxidomoybdato(VI)-k3 O:O′:O″)manganese(II)] C12H8N2O4MoMn
Ze-Hai, Qiu; Zhu-Sen, Zhang; Wu-Hua, Chen; Zeitschrift für Kristallographie - New Crystal Structures 236 (2021) 1347–1349; doi:10.1515/ncrs-2021-0338

data_8104604
_publ_section_title
;
 The crystal structure of catena-poly[(1,10-phenanthroline-k2
 N,N&#x2032;)-(\m3-tetraoxidomoybdato(VI)-k3
 O:O&#x2032;:O&#x2033;)manganese(II)] C12H8N2O4MoMn
;
_journal_issue                   6
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1347
_journal_page_last               1349
_journal_paper_doi               10.1515/ncrs-2021-0338
_journal_volume                  236
_journal_year                    2021
_chemical_formula_moiety         '0.5(C24 H16 Mn2 Mo2 N4 O8)'
_chemical_formula_sum            'C12 H8 Mn Mo N2 O4'
_chemical_formula_weight         395.08
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 100.120(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   8.9812(5)
_cell_length_b                   6.5212(3)
_cell_length_c                   10.6167(6)
_cell_measurement_reflns_used    1469
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.6100
_cell_measurement_theta_min      2.3130
_cell_volume                     612.13(6)
_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 0.992
_diffrn_measured_fraction_theta_max 0.841
_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    -68.00 -35.00   1.00    1.21    --  -17.60-178.00-150.00   33
  2  \w    -46.00  48.00   1.00    1.21    --  -17.60  19.00  90.00   94
  3  \w    -73.00   1.00   1.00    1.21    --  -17.60 -38.00  60.00   74
;
_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      0.0457737000
_diffrn_orient_matrix_UB_12      0.0131169000
_diffrn_orient_matrix_UB_13      -0.0475085000
_diffrn_orient_matrix_UB_21      0.0579133000
_diffrn_orient_matrix_UB_22      -0.0592966000
_diffrn_orient_matrix_UB_23      0.0371551000
_diffrn_orient_matrix_UB_31      -0.0313674000
_diffrn_orient_matrix_UB_32      -0.0901258000
_diffrn_orient_matrix_UB_33      -0.0312753000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0290
_diffrn_reflns_av_unetI/netI     0.0529
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.841
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2729
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.841
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         29.272
_diffrn_reflns_theta_min         1.949
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.069
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88163
_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 dark yellow'
_exptl_crystal_density_diffrn    2.144
_exptl_crystal_description       cube
_exptl_crystal_F_000             386
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.129
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1520
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.134
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0391
_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^)+(0.0096P)^2^+1.7057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0747
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1342
_reflns_number_total             1520
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2021-0338_suppl.cif
_cod_data_source_block           lym0912-d1
_cod_database_code               8104604
_chemical_oxdiff_formula         'C H N O Mo W Mn Co P V'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
O1 \\sim Mn1 \\sim Mo1: within 3.8A with sigma of 0.002 and sigma for terminal
atoms of 0.004
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10)
;