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_7046284
_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         'C18.04 H36.04 Mo3 N6 Na2 O18 S, 4(H2 O)'
_chemical_formula_sum            'C18.04 H44.04 Mo3 N6 Na2 O22 S'
_chemical_formula_weight         1062.97
_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             2018-04-10
_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                105.896(5)
_cell_angle_beta                 94.713(5)
_cell_angle_gamma                119.364(6)
_cell_formula_units_Z            2
_cell_length_a                   12.4659(7)
_cell_length_b                   12.7032(7)
_cell_length_c                   14.8254(9)
_cell_measurement_reflns_used    4322
_cell_measurement_temperature    173
_cell_measurement_theta_max      62.0368
_cell_measurement_theta_min      3.2056
_cell_volume                     1901.1(3)
_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    'ShelXS (Sheldrick, 2008)'
_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  -24.00   98.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -19.0000  -90.0000 122

  2 omega   47.00   95.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000  -30.0000 48

  3 omega   43.00   69.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000 -120.0000 26

  4 omega   52.00  104.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000 -180.0000 52

  5 omega   23.00   67.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -123.0000  -19.0000 44

  6 omega   26.00   63.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000   30.0000 37

  7 omega   73.00   99.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000  120.0000 26

  8 omega   51.00  116.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -38.0000   90.0000 65

  9 omega   74.00  128.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -25.0000   30.0000 54

 10 omega   91.00  167.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   77.0000   90.0000 76

 11 omega   79.00  117.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  112.0000 -120.0000 38

 12 omega   71.00   97.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  151.0000 -137.0000 26

 13 omega   47.00   78.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  178.0000  -90.0000 31

 14 omega   37.00  171.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   12.0000   60.0000 134

 15 omega   40.00   75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -99.0000  120.0000 35

 16 omega   23.00  105.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -50.0000   30.0000 82

 17 omega   32.00   58.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -25.0000   30.0000 26

 18 omega   21.00  127.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -93.0000   53.4868 106

 19 omega   22.00  132.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000  -90.0000 110

 20 omega   21.00   60.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000  -90.0000 39

 21 omega  -35.00   37.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -57.0000 -120.0000 72

 22 omega  -22.00   14.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -99.0000  120.0000 36

 23 omega -101.00  -74.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000 -120.0000 27

 24 omega -110.00  -70.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000  -30.0000 40

 25 omega -112.00  -75.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000   90.0000 37

 26 omega -113.00  -85.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066  178.0000 -150.0000 28
;
_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  0.0538
_diffrn_reflns_av_unetI/netI     0.0727
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10608
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        62.127
_diffrn_reflns_theta_max         62.127
_diffrn_reflns_theta_min         3.208
_exptl_absorpt_coefficient_mu    9.513
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41865
_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            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_description       plate
_exptl_crystal_F_000             1069
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.794
_refine_diff_density_min         -1.398
_refine_diff_density_rms         0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     520
_refine_ls_number_reflns         5910
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.138
_refine_ls_R_factor_all          0.0730
_refine_ls_R_factor_gt           0.0686
_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^)+(0.0821P)^2^+17.9074P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1790
_refine_ls_wR_factor_ref         0.1832
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5410
_reflns_number_total             5910
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00278a2.cif
_cod_data_source_block           exp_16981
_cod_depositor_comments
'Adding full bibliography for 7046283--7046286.cif.'
_cod_original_cell_volume        1901.1(2)
_cod_database_code               7046284
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H7A,H7B} of C7, {H1A,H1B} of C1, All C(H,H,H,H,H,H,H,H,H,
  H,H,H,H,H,H,H,H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
 At 2 times of:
  {H8WA,H8WB} of C15A
2. Restrained distances
 O2W-H2WB = O2W-H2WA
 0.85 with sigma of 0.01
 H2WA-H2WB
 1.39 with sigma of 0.01
 O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.01
 H1WA-H1WB
 1.39 with sigma of 0.01
 O3W-H3WA = O3W-H3WB
 0.9 with sigma of 0.01
 O7W-H7WA
 0.85 with sigma of 0.01
 O5W-H5WA = O5W-H5WB
 0.9 with sigma of 0.01
 H5WA-H5WB
 1.39 with sigma of 0.01
 O4W-H4WA = O4W-H4WB
 0.85 with sigma of 0.01
 H4WA-H4WB
 1.39 with sigma of 0.01
 O8W-H8WA
 0.85 with sigma of 0.01
 O10W-H10B = O10W-H10A
 0.85 with sigma of 0.01
 H10B-H10A
 1.39 with sigma of 0.01
 O9W-H9WA = O9W-H9WB
 0.85 with sigma of 0.01
 H9WA-H9WB
 1.39 with sigma of 0.01
 C15A-C13A \\sim C15-C13
 with sigma of 0.01
3. Rigid bond restraints
 C1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C15A \\sim C15 \\sim C13A \\sim C13: within 3.8A with sigma of 0.02 and sigma
for terminal atoms of 0.04
Uanis(C3A) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C9)
\\sim Ueq, Uanis(C15A) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C3A) \\sim Ueq, Uanis(C15) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.01
Uanis(C1) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C13A)
\\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5. Others
 Sof(H1B)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(H3AC)=1-FVAR(1)
 Sof(H1A)=Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(H3C)=FVAR(1)
 Sof(H7B)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=1-FVAR(2)
 Sof(H7A)=Sof(C9)=Sof(H9A)=Sof(H9B)=Sof(H9C)=FVAR(2)
 Sof(C13A)=Sof(H13A)=FVAR(3)
 Fixed Sof: C13(0.46) H13(0.46) C15(0.6) H15A(0.6) H15B(0.6) H15C(0.6)
 C15A(0.4) H15D(0.4) H15E(0.4) H15F(0.4)
6.a Riding coordinates:
 C15A(H9WA,H9WB,H10A,H10B,H8WA,H4WA,H4WB,H7WA,H5WA,H5WB,H7WB,H8WB,H6WA,H6WB,
 H3WA,H3WB,H1WA,H1WB)
6.b Ternary CH refined with riding coordinates:
 C7(H7A), C7(H7B), C1(H1A), C1(H1B), C13(H13), C13A(H13A)
6.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N6(H6), N4(H4), C6(H6A), C4(H4A), C16(H16), C18(H18), C11(H11),
 C17(H17), C12(H12), C10(H10), C5(H5)
6.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC), C15(H15A,H15B,H15C), C9(H9A,H9B,H9C),
 C9A(H9AA,H9AB,H9AC), C15A(H15D,H15E,H15F)
;
_shelx_res_checksum              98786
_olex2_exptl_crystal_mounting_method set
_olex2_submission_special_instructions 'No special instructions were received'