Molybdenum imidazole citrate and bipyridine homocitrate in different oxidation states ‒ balance between coordinated α-hydroxy and α-alkoxy groups
Wang, Si-Yuan; Zhou, Zhao-Hui; RSC Advances 9 (2019) 519–; doi:10.1039/C8RA09134J

data_7232150
_publ_section_title
;
 Molybdenum imidazole citrate and bipyridine homocitrate in different
 oxidation states -- balance between coordinated \a-hydroxy and \a-alkoxy
 groups
;
_journal_issue                   1
_journal_name_full               'RSC Advances'
_journal_page_first              519
_journal_paper_doi               10.1039/C8RA09134J
_journal_volume                  9
_journal_year                    2019
_chemical_formula_moiety
'C21 H22 Mo5 N6 O23 S, 2(C3 H5 N2), 6(H2 O), C3 H4 N2'
_chemical_formula_sum            'C30 H48 Mo5 N12 O29 S'
_chemical_formula_weight         1552.53
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-14
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-04-16 deposited with the CCDC.
2018-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.660(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.9484(4)
_cell_length_b                   15.2878(3)
_cell_length_c                   15.5230(3)
_cell_measurement_reflns_used    9543
_cell_measurement_temperature    173
_cell_measurement_theta_max      62.0939
_cell_measurement_theta_min      3.1612
_cell_volume                     5061.30(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_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      173
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details
;
  1 omega   34.00  102.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       32.3066   57.0000   60.0000 68

  2 omega   73.00  166.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   50.0000  120.0000 93

  3 omega  105.00  165.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   50.0000  150.0000 60

  4 omega   79.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  112.0000   30.0000 26

  5 omega   49.00   81.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  178.0000   90.0000 32

  6 omega   39.00  102.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  178.0000  150.0000 63

  7 omega   36.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  178.0000  -60.0000 33

  8 omega   79.00  120.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   38.0000 -150.0000 41

  9 omega  121.00  147.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   38.0000 -150.0000 26

 10 omega   26.00  121.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -64.0000  -30.0000 95

 11 omega   34.00   76.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000  150.0000 42

 12 omega   27.00  118.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -50.0000  120.0000 91

 13 omega   21.00   47.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000   60.0000 26

 14 omega  -33.00  100.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       32.3066   19.0000 -120.0000 133

 15 omega  -99.00  -74.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000   60.0000 25
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0024643000
_diffrn_orient_matrix_UB_12      0.0678761000
_diffrn_orient_matrix_UB_13      0.0722576000
_diffrn_orient_matrix_UB_21      0.0692780000
_diffrn_orient_matrix_UB_22      -0.0190498000
_diffrn_orient_matrix_UB_23      0.0446171000
_diffrn_orient_matrix_UB_31      0.0205113000
_diffrn_orient_matrix_UB_32      0.0719341000
_diffrn_orient_matrix_UB_33      -0.0567175000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_unetI/netI     0.0422
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            16632
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        62.184
_diffrn_reflns_theta_max         62.184
_diffrn_reflns_theta_min         3.557
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    11.190
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    2.030
_exptl_crystal_description       plate
_exptl_crystal_F_000             3056
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.759
_refine_diff_density_min         -1.538
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         7914
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0611P)^2^+32.8388P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1137
_refine_ls_wR_factor_ref         0.1153
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7547
_reflns_number_total             7914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra09134j2.cif
_cod_data_source_block           exp_16371
_cod_database_code               7232150
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.90
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H5WA,H5WB} of O5WB, All C(H,H) groups, All C(H,H,H,H)
  groups, All N(H) groups, All O(H,H,H,H,H,H,H,H,H,H) groups
 At 1.5 times of:
  {H5WC,H5WD} of O5WA
2. Restrained distances
 N7-H7 = N9-H9 = N10-H10
 0.86 with sigma of 0.01
 H10-C26 = H10-C25
 2 with sigma of 0.01
 H1WA-O1W = H1WB-O1W = H2WA-O2W = H2WB-O2W = H3WA-O3W = H3WB-O3W = H4WA-O4W =
 H4WB-O4W
 0.85 with sigma of 0.01
 H1WA-H1WB = H2WA-H2WB = H4WB-H4WA
 1.39 with sigma of 0.01
 O20-N11
 3 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O6W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Sof(O5WB)=Sof(H5WA)=Sof(H5WB)=1-FVAR(1)
 Sof(O5WA)=Sof(H5WC)=Sof(H5WD)=FVAR(1)
5.a Riding coordinates:
 C27(H27), C26(H26), C25(H25), C25(H7,H9,H10), O6W(H1WA,H2WA,H2WB,H3WA,H4WA,
 H4WB,H3WB,H6WA,H6WB,H1WB), O5WB(H5WA,H5WB), O5WA(H5WC,H5WD)
5.b Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C11(H11A,H11B), C3(H3A,H3B), C5(H5A,H5B)
5.c Aromatic/amide H refined with riding coordinates:
 N6(H6), N2(H2), C19(H19), N8(H8), N4(H4), C18(H18), C15(H15), C13(H13),
 C22(H22), C17(H17), C20(H20), C21(H21), C14(H14), C16(H16), C24(H24), C23(H23)
;
_olex2_submission_special_instructions 'No special instructions were received'