Molybdenum-maltolate as a molybdopterin mimic for bioinspired oxidation reaction.
Pawar, Swapnil S.; Ketkar, Rohit N.; Gaware, Pranav B.; Jagushte, Kaustubh U.; Dhawne, Divyani; Save, Shreyada N.; Sharma, Shilpy; Periyasamy, Ganga; Chimthanawala, Niyamat; Sathaye, Sadhana; Joshi, Shreerang V.; Sadhukhan, Nabanita; Dalton transactions (Cambridge, England : 2003) 53 (2024) 5770–5774; doi:10.1039/d3dt04296k

data_7715078
_publ_section_title
;
 Molybdenum-maltolate as a molybdopterin mimic for bioinspired oxidation
 reaction.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5770
_journal_page_last               5774
_journal_paper_doi               10.1039/d3dt04296k
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C6 H6 O3'
_chemical_formula_sum            'C6 H6 O3'
_chemical_formula_weight         126.11
_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   geom
_atom_sites_solution_primary     dual
_audit_block_doi                 10.5517/ccdc.csd.cc2gyqtz
_audit_update_record
;
2023-09-04 deposited with the CCDC.	2024-01-19 downloaded from the CCDC.
;
_cell_angle_alpha                85.419(4)
_cell_angle_beta                 86.684(4)
_cell_angle_gamma                70.931(5)
_cell_formula_units_Z            10
_cell_length_a                   6.9493(4)
_cell_length_b                   7.1414(4)
_cell_length_c                   30.2196(13)
_cell_measurement_reflns_used    4476
_cell_measurement_temperature    150
_cell_measurement_theta_max      72.8690
_cell_measurement_theta_min      5.9560
_cell_volume                     1412.10(14)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_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      150
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.948
_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   -191.00 -11.00   1.00    4.00    -- -101.00   0.00  36.00  180
  2  \w   -122.00  27.00   1.00    4.00    --  -32.00   0.00-108.00  149
  3  \w   -107.00 -11.00   1.00    4.00    -- -101.00  72.00 -36.00   96
  4  \w   -105.00 -27.00   1.00    4.00    -- -101.00  72.00 144.00   78
  5  \w   -106.00 -22.00   1.00    4.00    -- -101.00  72.00-144.00   84
  6  \w   -120.00 -34.00   1.00    4.00    -- -101.00  43.00 108.00   86
  7  \w    -58.00  15.00   1.00    4.00    --  -32.00  72.00-108.00   73
  8  \w    -97.00 -67.00   1.00    4.00    -- -101.00  72.00  72.00   30
  9  \w    -66.00 -16.00   1.00    4.00    --  -32.00  72.00 108.00   50
 10  \w   -106.00 -22.00   1.00    4.00    -- -101.00  72.00 -72.00   84
 11  \w   -106.00 -76.00   1.00    4.00    -- -101.00  72.00  36.00   30
 12  \w    -94.00 -19.00   1.00    4.00    -- -101.00  72.00 108.00   75
 13  \w   -162.00 -77.00   1.00    4.00    -- -101.00 -44.00 144.00   85
 14  \w    -97.00 -31.00   1.00    4.00    -- -101.00  72.00-108.00   66
 15  \w   -155.00-111.00   1.00    4.00    -- -101.00 -72.00 108.00   44
 16  \w    -44.00 -14.00   1.00    4.00    --  -32.00  72.00 -36.00   30
 17  \w   -120.00 -89.00   1.00    4.00    -- -101.00  72.00   0.00   31
 18  \w   -117.00 -86.00   1.00    4.00    -- -101.00  72.00-180.00   31
 19  \w   -191.00 -67.00   1.00    4.00    -- -101.00 -72.00  36.00  124
 20  \w   -191.00 -67.00   1.00    4.00    -- -101.00 -72.00 -36.00  124
 21  \w   -191.00 -67.00   1.00    4.00    -- -101.00 -72.00-108.00  124
 22  \w   -122.00  58.00   1.00    4.00    --  -32.00   0.00  36.00  180
 23  \w   -191.00 -70.00   1.00    4.00    -- -101.00 -72.00 144.00  121
 24  \w   -191.00-184.00   1.00    4.00    -- -101.00 -72.00  72.00    7
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1794852000
_diffrn_orient_matrix_UB_12      -0.0439390000
_diffrn_orient_matrix_UB_13      0.0259712000
_diffrn_orient_matrix_UB_21      0.0227919000
_diffrn_orient_matrix_UB_22      0.1230309000
_diffrn_orient_matrix_UB_23      0.0377900000
_diffrn_orient_matrix_UB_31      -0.1494842000
_diffrn_orient_matrix_UB_32      0.1877467000
_diffrn_orient_matrix_UB_33      -0.0227141000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1271
_diffrn_reflns_av_unetI/netI     0.1016
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.948
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            18978
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.948
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.895
_diffrn_reflns_theta_min         2.936
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.031
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.59571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_description       block
_exptl_crystal_F_000             660
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0907
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2389
_refine_ls_wR_factor_ref         0.3199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3551
_reflns_number_total             5419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt04296k2.cif
_cod_data_source_block           Maltol
_cod_depositor_comments
;
Adding full bibliography for 7715077--7715078.cif.

2024-06-28
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C30 H30 O15'
_cod_original_formula_weight         630.54
_cod_original_formula_moiety         '5(C6 H6 O3)'
_cod_original_formula_units_Z            2
_cod_original_cell_volume        1412.09(13)
_cod_database_code               7715078
_chemical_oxdiff_formula         C6O3H10
_shelx_estimated_absorpt_t_max   0.945
_shelx_estimated_absorpt_t_min   0.783
_reflns_odcompleteness_completeness 94.82
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     73.73
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C9(H9), C10(H10), C15(H15), C16(H16), C21(H21), C22(H22),
 C27(H27), C28(H28)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C12(H12A,H12B,H12C), C18(H18A,H18B,H18C), C24(H24A,H24B,
 H24C), C30(H30A,H30B,H30C)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2), O5(H5), O8(H8), O11(H11), O14(H14)
;
_shelx_res_checksum              57055
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.469
_oxdiff_exptl_absorpt_empirical_full_min 0.392