Comparison of hydroxycarboxylato imidazole molybdenum(iv) complexes and nitrogenase protein structures: indirect evidence for the protonation of homocitrato FeMo-cofactors.
Wang, Si-Yuan; Jin, Wan-Ting; Chen, Hong-Bin; Zhou, Zhao-Hui; Dalton transactions (Cambridge, England : 2003) 47 (2018) 7412–7421; doi:10.1039/c8dt00278a

data_7046283
_publ_section_title
;
 Comparison of hydroxycarboxylato imidazole molybdenum(iv) complexes and
 nitrogenase protein structures: indirect evidence for the protonation of
 homocitrato FeMo-cofactors.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7412
_journal_page_last               7421
_journal_paper_doi               10.1039/c8dt00278a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C19 H24 Mo3 N10 O9 S'
_chemical_formula_sum            'C19 H24 Mo3 N10 O9 S'
_chemical_formula_weight         856.36
_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     dual
_audit_creation_date             2018-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-04-13 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                109.173(3)
_cell_angle_beta                 104.625(3)
_cell_angle_gamma                90.077(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6290(3)
_cell_length_b                   12.1305(4)
_cell_length_c                   17.0785(6)
_cell_measurement_reflns_used    6830
_cell_measurement_temperature    173
_cell_measurement_theta_max      28.6780
_cell_measurement_theta_min      2.5020
_cell_volume                     1626.85(11)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_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                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1903
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.893
_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    -59.00  10.00   1.00   22.50    --  -22.85 -77.00 -90.00   69
  2  \w    -91.00  31.00   1.00   22.50    --  -22.85 -19.00 150.00  122
  3  \w    -93.00 -65.00   1.00   22.50    --  -22.85 -57.00 150.00   28
  4  \w    -47.00  -1.00   1.00   22.50    --  -22.85 -57.00 150.00   46
  5  \w    -55.00  40.00   1.00   22.50    --  -22.85  77.00-150.00   95
  6  \w    -47.00  40.00   1.00   22.50    --  -22.85  57.00 -30.00   87
  7  \w    -51.00  50.00   1.00   22.50    --  -22.85  77.00 120.00  101
  8  \w    -92.00  10.00   1.00   22.50    --  -22.85 -77.00  90.00  102
  9  \w    -77.00  -2.00   1.00   22.50    --  -22.85 -57.00 -30.00   75
 10  \w     -4.00  69.00   1.00   22.50    --   24.10 -99.00  60.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0564673000
_diffrn_orient_matrix_UB_12      0.0500537000
_diffrn_orient_matrix_UB_13      0.0164092000
_diffrn_orient_matrix_UB_21      -0.0550534000
_diffrn_orient_matrix_UB_22      0.0289608000
_diffrn_orient_matrix_UB_23      -0.0232158000
_diffrn_orient_matrix_UB_31      -0.0325448000
_diffrn_orient_matrix_UB_32      0.0228268000
_diffrn_orient_matrix_UB_33      0.0357004000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0552
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.893
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            25698
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.893
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.916
_diffrn_reflns_theta_min         2.449
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.261
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91791
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.748
_exptl_crystal_description       needle
_exptl_crystal_F_000             844
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.999
_refine_diff_density_min         -0.843
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         8418
_refine_ls_number_restraints     181
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0396P)^2^+0.1148P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0913
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6895
_reflns_number_total             8418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00278a2.cif
_cod_data_source_block           exp_17643
_cod_depositor_comments
'Adding full bibliography for 7046283--7046286.cif.'
_cod_original_cell_volume        1626.85(10)
_cod_database_code               7046283
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.951
_shelx_estimated_absorpt_t_min   0.704
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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 N(H,H) groups
2. Restrained distances
 N8-H8
 0.88 with sigma of 0.01
 N4-H4
 0.88 with sigma of 0.01
 N1-C5 \\sim N1-C5A
 with sigma of 0.02
 C4-C5 \\sim C4-C5A
 with sigma of 0.02
 N2-C4 \\sim N2-C4A
 with sigma of 0.02
 C4-C5 \\sim C4A-C5
 with sigma of 0.02
 C4-C5A \\sim C4A-C5A
 with sigma of 0.02
 C4A-C5A \\sim C4-C5
 with sigma of 0.01
3. Rigid bond restraints
 O5, C2, O7, C6, N1, N3, C10, N6, C12, N9, C19, N10, C18, C4, N2, N2, C3
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O3 \\sim O2 \\sim O1 \\sim O4 \\sim O5 \\sim O8 \\sim O7 \\sim O6 \\sim O9:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.01
C4 \\sim C4A \\sim C5 \\sim C5A: within 3.8A with sigma of 0.02 and sigma for
terminal atoms of 0.04
Uanis(C1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C9) \\sim
Ueq, Uanis(C18) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of
0.01
5. Others
 Sof(H2B)=Sof(C4A)=Sof(H4AA)=1-FVAR(1)
 Sof(H2A)=Sof(C4)=Sof(H4A)=FVAR(1)
 Fixed Sof: C5(0.7) H5(0.7) C5A(0.3) H5A(0.3)
6.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C6(H6A,H6B)
6.b Aromatic/amide H refined with riding coordinates:
 N2(H2A), N2(H2B), N6(H6), N10(H10), C14(H14), C12(H12), C8(H8A), C17(H17),
 C3(H3), C4(H4A), C11(H11), C13(H13), C16(H16), C15(H15), C9(H9), C19(H19),
 C10(H10A), C18(H18), C5(H5), C5A(H5A), C4A(H4AA)
;
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 1.138
_oxdiff_exptl_absorpt_empirical_full_min 0.893