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_7046285
_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         '0.5(C32 H24 Mo12 Na12 O64)'
_chemical_formula_sum            'C16 H12 Mo6 Na6 O32'
_chemical_formula_weight         1429.84
_space_group_crystal_system      orthorhombic
_space_group_IT_number           44
_space_group_name_Hall           'I 2 -2'
_space_group_name_H-M_alt        'I m m 2'
_symmetry_space_group_name_Hall  'I 2 -2'
_symmetry_space_group_name_H-M   'I m m 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-04-13
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.0786(10)
_cell_length_b                   18.8242(10)
_cell_length_c                   7.2176(5)
_cell_measurement_reflns_used    2274
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      62.0955
_cell_measurement_theta_min      3.7528
_cell_volume                     2048.7(2)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega -105.00  -74.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000   90.0000 31

  2 omega -104.00  -58.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066 -178.0000  -90.0000 46

  3 omega  -75.00  -39.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066   97.0000  115.0000 36

  4 omega -113.00  -69.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -      -32.3066  178.0000 -180.0000 44

  5 omega  -42.00   72.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -19.0000  150.0000 114

  6 omega  -38.00   26.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -57.0000  -60.0000 64

  7 omega  -39.00   64.00   1.0000    2.5000
omega____ theta____ kappa____ phi______ frames
    -       32.3066  -38.0000   60.0000 103

  8 omega   23.00   49.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -50.0000 -150.0000 26

  9 omega   23.00   91.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000  150.0000 68

 10 omega   74.00  101.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -50.0000  120.0000 27

 11 omega   68.00  162.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   64.0000  -90.0000 94

 12 omega  115.00  165.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   50.0000 -150.0000 50

 13 omega   71.00   99.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000 -120.0000 28

 14 omega  117.00  153.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   64.0000 -120.0000 36

 15 omega   99.00  169.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   25.0000  -30.0000 70

 16 omega   32.00   67.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000 -112.0000 -150.0000 35

 17 omega   27.00  136.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000  -30.0000 109

 18 omega   53.00  120.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -50.0000 -150.0000 67

 19 omega   64.00  168.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000   38.0000   30.0000 104

 20 omega   83.00  132.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -92.0000  120.0000 49

 21 omega   34.00  120.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -50.0000  -30.0000 86

 22 omega   24.00   53.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -50.0000  120.0000 29

 23 omega  102.00  134.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  112.0000  -30.0000 32

 24 omega   74.00  101.00   1.0000    8.0000
omega____ theta____ kappa____ phi______ frames
    -       94.5000  -93.0000 -151.7662 27
;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0399832000
_diffrn_orient_matrix_UB_12      0.0884728000
_diffrn_orient_matrix_UB_13      -0.0378755000
_diffrn_orient_matrix_UB_21      -0.0623435000
_diffrn_orient_matrix_UB_22      -0.0510719000
_diffrn_orient_matrix_UB_23      -0.0667095000
_diffrn_orient_matrix_UB_31      -0.2001062000
_diffrn_orient_matrix_UB_32      -0.0020187000
_diffrn_orient_matrix_UB_33      0.0285808000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_unetI/netI     0.0416
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       5
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5531
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        62.185
_diffrn_reflns_theta_max         62.185
_diffrn_reflns_theta_min         3.756
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    16.168
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22525
_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    2.318
_exptl_crystal_description       needle
_exptl_crystal_F_000             1364
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.745
_refine_diff_density_min         -1.161
_refine_diff_density_rms         0.215
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.03(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         1451
_refine_ls_number_restraints     153
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.071
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1163P)^2^+15.2479P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1511
_refine_ls_wR_factor_ref         0.1541
_reflns_Friedel_coverage         0.837
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                1405
_reflns_number_total             1451
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00278a2.cif
_cod_data_source_block           exp_15827
_cod_depositor_comments
'Adding full bibliography for 7046283--7046286.cif.'
_cod_database_code               7046285
_shelx_shelxl_version_number     2014/7
_reflns_odcompleteness_completeness 99.89
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     61.08
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.97(6)
 0.03(6)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
3. Rigid bond restraints
 O2, C2, Mo2, O1
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 O5, C4, O4, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
4. Uiso/Uaniso restraints and constraints
C1 \\sim C3 \\sim C4 \\sim C2: within 3.8A with sigma of 0.005 and sigma for
terminal atoms of 0.01
O1 \\sim O10 \\sim O9 \\sim O7 \\sim O2 \\sim O5 \\sim O8 \\sim O3 \\sim O4
\\sim O6: within 3.8A with sigma of 0.005 and sigma for terminal atoms of 0.01
5.a Ternary CH refined with riding coordinates:
 C1(H1)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B)
;
_olex2_submission_special_instructions 'No special instructions were received'