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_7232149
_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 H24 K2 Mo5 N6 O25, 3(C3 H4 N2), 1.5(H4 O2)'
_chemical_formula_sum            'C30 H42 K2 Mo5 N12 O28'
_chemical_formula_weight         1576.62
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-03-13
_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                100.570(4)
_cell_angle_beta                 94.254(3)
_cell_angle_gamma                101.331(4)
_cell_formula_units_Z            2
_cell_length_a                   9.7975(3)
_cell_length_b                   13.8912(7)
_cell_length_c                   18.5268(8)
_cell_measurement_reflns_used    7524
_cell_measurement_temperature    173
_cell_measurement_theta_max      62.0726
_cell_measurement_theta_min      3.3107
_cell_volume                     2414.44(18)
_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    'SIR2004 (Burla et al., 2007)'
_diffrn_ambient_temperature      173.0
_diffrn_detector_area_resol_mean 16.1903
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_details
;
  1 omega    7.00   56.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -57.0000   90.0000 49

  2 omega   21.00   60.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000  -30.0000 39

  3 omega   25.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000  -60.0000 66

  4 omega   76.00  103.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000 -120.0000 27

  5 omega   50.00   91.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000 -180.0000 41

  6 omega   51.00   98.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000 -180.0000 47

  7 omega   43.00   72.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -99.0000 -180.0000 29

  8 omega   38.00  103.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -50.0000  -60.0000 65

  9 omega   34.00   61.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000 -120.0000 27

 10 omega   23.00  113.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000  -30.0000 90

 11 omega   73.00  102.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000   90.0000 29

 12 omega   31.00  167.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000    0.0000   90.0000 136

 13 omega  124.00  151.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   64.0000  150.0000 27

 14 omega  117.00  144.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   50.0000   90.0000 27

 15 omega   81.00  164.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   50.0000  120.0000 83

 16 omega   75.00  110.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   50.0000   90.0000 35

 17 omega   68.00  101.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   64.0000  150.0000 33

 18 omega   23.00  120.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -38.0000  120.0000 97

 19 omega   25.00   52.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000   60.0000 27

 20 omega   24.00  104.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -64.0000   30.0000 80

 21 omega  -16.00   35.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -99.0000 -180.0000 51

 22 omega  -94.00  -66.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000 -150.0000 28

 23 omega -105.00  -63.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000  -30.0000 42

 24 omega  -36.00  106.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -       32.3066    0.0000  150.0000 142

 25 omega  -92.00  -61.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000  120.0000 31

 26 omega -104.00   -5.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066  -77.0000    0.0000 99

 27 omega -113.00  -63.00   1.0000    4.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066  178.0000 -180.0000 50
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0337
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13938
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        62.162
_diffrn_reflns_theta_max         62.162
_diffrn_reflns_theta_min         3.313
_exptl_absorpt_coefficient_mu    12.849
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.55775
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.163
_exptl_crystal_description       needle
_exptl_crystal_F_000             1548
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.04
_refine_diff_density_max         2.989
_refine_diff_density_min         -1.466
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     685
_refine_ls_number_reflns         7516
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0711P)^2^+15.2223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1276
_refine_ls_wR_factor_ref         0.1299
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7068
_reflns_number_total             7516
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra09134j2.cif
_cod_data_source_block           exp_16411
_cod_database_code               7232149
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups, All O(H,H) groups, All
  O(H,H,H) groups, All O(H,H,H,H,H,H) groups
2. Restrained distances
 N11-C28
 1.38 with sigma of 0.01
 N12-C28
 1.32 with sigma of 0.01
 N11-C30 = N12-C29
 1.36 with sigma of 0.01
 C29-C30
 1.35 with sigma of 0.01
 C28-C30
 2.2 with sigma of 0.01
 N7-N9
 3.1 with sigma of 0.01
 O1-H1 = O11-H11 = H1WA-O1W = H1WB-O1W = H3WA-O3W = H3WB-O3W = H2WA-O2W = H2WB-
 O2W
 0.85 with sigma of 0.01
 H1WA-H1WB = H3WA-H3WB = H2WA-H2WB
 1.39 with sigma of 0.01
 N10-H10
 0.88 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O1W) \\sim Ueq, Uanis(O3W) \\sim Ueq, Uanis(O2W) \\sim Ueq, Uanis(C14)
\\sim Ueq, Uanis(O4WA) \\sim Ueq, Uanis(O4WB) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4. Others
 Sof(O4WB)=Sof(H4WC)=Sof(H4WD)=1-FVAR(1)
 Sof(O4WA)=Sof(H4WA)=Sof(H4WB)=FVAR(1)
5.a Riding coordinates:
 O3W(H1WA,H1WB,H3WA,H3WB,H2WA,H2WB), O4WA(H4WA,H4WB), O4WB(H10), O4WB(H4WC,H4WD)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C5(H5A,H5B), C9(H9A,H9B), C11(H11A,H11B)
5.c Aromatic/amide H refined with riding coordinates:
 N4(H4), N6(H6), N8(H8), C16(H16), C23(H23), C19(H19), C24(H24), C21(H21),
 C13(H13), C14(H14), C15(H15), C22(H22), C20(H20), C18(H18), C17(H17), C27(H27),
  N2(H2), C25(H25), C26(H26)
;
_olex2_submission_special_instructions 'No special instructions were received'