Crystal structure of tetrakis(1H-benzo[d]imidazol-3-ium) bis(μ5-phenylphosphonato)-pentakis(μ2-oxido)-decaoxo-penta-molybdenum dihydrate, C40H42Mo5N8O23P2
Ma, Feng-Xia; Jiang, Jin-Ke; Yuan, Yuan; Li, Dong-Dong; Zeitschrift für Kristallographie - New Crystal Structures 235 (2020) 1191–1193; doi:10.1515/ncrs-2020-0245

data_8105418
_publ_section_title
;
 Crystal structure of tetrakis(1H-benzo[d]imidazol-3-ium)
 bis(\m5-phenylphosphonato)-pentakis(\m2-oxido)-decaoxo-penta-molybdenum
 dihydrate, C40H42Mo5N8O23P2
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              1191
_journal_page_last               1193
_journal_paper_doi               10.1515/ncrs-2020-0245
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         'C12 H10 Mo5 O21 P2, 2(H2 O), 4(C7 H7 N2)'
_chemical_formula_sum            'C40 H42 Mo5 N8 O23 P2'
_chemical_formula_weight         1544.45
_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                85.583(2)
_cell_angle_beta                 81.294(2)
_cell_angle_gamma                84.844(2)
_cell_formula_units_Z            2
_cell_length_a                   10.9867(2)
_cell_length_b                   15.4753(3)
_cell_length_c                   15.5666(3)
_cell_measurement_reflns_used    21969
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.8940
_cell_measurement_theta_min      5.0640
_cell_volume                     2600.18(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.7e (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.992
_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    -18.00  12.00   0.50    1.49    --   -0.40  38.00-120.00   60
  2  \w     -4.00  23.00   0.50    1.49    --   -0.40  77.00 -90.00   54
  3  \w     35.00  81.00   0.50    1.49    --   -0.40  77.00 -90.00   92
  4  \w     26.00  89.00   0.50    1.49    --   -0.40  77.00-180.00  126
  5  \w      7.00  34.00   0.50    1.49    --   -0.40  77.00  60.00   54
  6  \w    -27.00  37.00   0.50    1.49    --   -0.40  77.00-120.00  128
  7  \w    -57.00  17.00   0.50    1.49    --   -0.40 -38.00-150.00  148
  8  \w     -6.00  19.00   0.50    1.49    --   -0.40 -57.00-180.00   50
  9  \w     -8.00  17.00   0.50    1.49    --   -0.40 -57.00 -90.00   50
 10  \w    -43.00 -16.00   0.50    1.49    --   -0.40 -57.00 -90.00   54
 11  \w    -75.00  15.00   0.50    1.49    --   -0.40 -38.00  60.00  180
 12  \w    -90.00 -34.00   0.50    1.49    --   -0.40 -57.00-180.00  112
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Pro: Kappa dual offset/far'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0139037000
_diffrn_orient_matrix_UB_12      0.0297575000
_diffrn_orient_matrix_UB_13      -0.0348160000
_diffrn_orient_matrix_UB_21      -0.0307148000
_diffrn_orient_matrix_UB_22      0.0295172000
_diffrn_orient_matrix_UB_23      0.0303574000
_diffrn_orient_matrix_UB_31      0.0561789000
_diffrn_orient_matrix_UB_32      0.0192342000
_diffrn_orient_matrix_UB_33      0.0001442000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0274
_diffrn_reflns_av_unetI/netI     0.0203
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            47853
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         4.922
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.324
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83400
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.7e (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.973
_exptl_crystal_description       Block
_exptl_crystal_F_000             1524
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.442
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         10563
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0271
_refine_ls_R_factor_gt           0.0208
_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^)+(0.0149P)^2^+2.7145P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0485
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9260
_reflns_number_total             10563
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2020-0245_suppl.cif
_cod_data_source_block           2
_cod_database_code               8105418
_shelx_estimated_absorpt_t_max   0.857
_shelx_estimated_absorpt_t_min   0.826
_reflns_odcompleteness_completeness 99.24
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1W-H1WA = H2WA-O2W
 0.9 with sigma of 0.02
 H1WA-H2WA
 2.1 with sigma of 0.01
 H2WA-H1WA
 2.15 with sigma of 0.01
 O2W-H2WA
 0.85 with sigma of 0.02
 H2WB-O2W
 0.9 with sigma of 0.01
 H2WA-H2WB
 1.37 with sigma of 0.01
3.a Aromatic/amide H refined with riding coordinates:
 C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C36(H36), C37(H37),
 C38(H38), C39(H39), C40(H40), N1(H1), N2(H2), C1(H1A), C2(H2A), C3(H3), C4(H4),
  C7(H7), N3(H3A), N4(H4A), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14),
 N5(H5), N6(H6), C15(H15), C16(H16), C17(H17), C18(H18), C21(H21), N7(H7A),
 N8(H8A), C22(H22), C23(H23), C24(H24), C27(H27), C28(H28)
;