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_7046286
_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         'C36 H50 Mo6 N20 O16'
_chemical_formula_sum            'C36 H50 Mo6 N20 O16'
_chemical_formula_weight         1594.60
_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             2018-04-13
_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                90.197(4)
_cell_angle_beta                 106.313(5)
_cell_angle_gamma                110.829(4)
_cell_formula_units_Z            1
_cell_length_a                   10.6194(5)
_cell_length_b                   11.9177(5)
_cell_length_c                   14.7094(10)
_cell_measurement_reflns_used    2311
_cell_measurement_temperature    173
_cell_measurement_theta_max      25.5550
_cell_measurement_theta_min      2.9070
_cell_volume                     1658.78(17)
_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 0.999
_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      7.00  73.00   1.00   26.00    --   24.10  57.00 -60.00   66
  2  \w     51.00  81.00   1.00   26.00    --   24.10-129.00 119.00   30
  3  \w     68.00  95.00   1.00   26.00    --   24.10-143.00 -51.00   27
  4  \w    -73.00 -44.00   1.00   26.00    --  -22.85-178.00  60.00   29
  5  \w    -95.00 -35.00   1.00   26.00    --  -22.85-178.00  90.00   60
  6  \w    -96.00   7.00   1.00   26.00    --  -22.85 -38.00 -60.00  103
  7  \w    -96.00   8.00   1.00   26.00    --  -22.85 -38.00  30.00  104
  8  \w   -104.00 -78.00   1.00   26.00    --  -22.85 178.00-180.00   26
;
_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      0.0088040000
_diffrn_orient_matrix_UB_12      0.0032397000
_diffrn_orient_matrix_UB_13      -0.0460913000
_diffrn_orient_matrix_UB_21      0.0740253000
_diffrn_orient_matrix_UB_22      0.0171863000
_diffrn_orient_matrix_UB_23      0.0206530000
_diffrn_orient_matrix_UB_31      -0.0078557000
_diffrn_orient_matrix_UB_32      -0.0616733000
_diffrn_orient_matrix_UB_33      -0.0027214000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0794
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11292
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.152
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.167
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.98843
_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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.596
_exptl_crystal_description       plate
_exptl_crystal_F_000             786
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.153
_refine_diff_density_min         -1.031
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5853
_refine_ls_number_restraints     419
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0493P)^2^+0.3511P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1138
_refine_ls_wR_factor_ref         0.1199
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4536
_reflns_number_total             5853
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00278a2.cif
_cod_data_source_block           exp_17169
_cod_depositor_comments
'Adding full bibliography for 7046283--7046286.cif.'
_cod_original_cell_volume        1658.78(16)
_cod_database_code               7046286
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.800
_reflns_odcompleteness_completeness 99.92
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N10-H10A
 0.88 with sigma of 0.01
 O6-H6A
 0.85 with sigma of 0.01
 C2-C1
 1.5 with sigma of 0.01
3. Rigid bond restraints
 C1, C3A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 O6, C1, Mo3, N7
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.0025
 Mo3, O3
 with sigma for 1-2 distances of 0.00125 and sigma for 1-3 distances of 0.000625
 C18, C17, C17, N10, N10, C16, C15, C14, C14, N8, N8, C13, C2, O7, C2, O8, C1,
 C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C18 \\sim C17 \\sim C17 \\sim N10 \\sim N10 \\sim C16 \\sim C15 \\sim C14 \\sim
C14 \\sim N8 \\sim N8 \\sim C13 \\sim C2 \\sim O7 \\sim C2 \\sim O8 \\sim C1
\\sim C2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C7 \\sim C10 \\sim C4 \\sim C9 \\sim C12 \\sim C11 \\sim C2 \\sim C8 \\sim C6
\\sim C16 \\sim C15 \\sim C18 \\sim C5 \\sim C13 \\sim C17 \\sim C1 \\sim C14
\\sim C3 \\sim C3A: within 3.8A with sigma of 0.01 and sigma for terminal atoms
of 0.02
N3 \\sim N5 \\sim N1 \\sim N4 \\sim N9 \\sim N6 \\sim N7 \\sim N2 \\sim N8
\\sim N10: within 3.8A with sigma of 0.005 and sigma for terminal atoms of 0.01
O2 \\sim O5 \\sim O1 \\sim O3 \\sim O4 \\sim O7 \\sim O8 \\sim O6: within 3.8A
with sigma of 0.0025 and sigma for terminal atoms of 0.005
Uanis(C3) \\sim Ueq, Uanis(C3A) \\sim Ueq, Uanis(C2) \\sim Ueq: with sigma of
0.02 and sigma for terminal atoms of 0.01
Uanis(N8) \\sim Ueq, Uanis(N10) \\sim Ueq: with sigma of 0.005 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)
6.a Riding coordinates:
 C3A(H6A)
6.b Ternary CH refined with riding coordinates:
 C1(H1A), C1(H1B)
6.c Aromatic/amide H refined with riding coordinates:
 N4(H4), N6(H6), C7(H7), N2(H2), C10(H10), C4(H4A), C9(H9), C12(H12), C11(H11),
  C8(H8), C6(H6B), C16(H16), C15(H15), C18(H18), C5(H5), C13(H13), C17(H17),
 N8(H8A), N10(H10A), C14(H14)
6.d Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C3A(H3AA,H3AB,H3AC)
;
_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 1.125
_oxdiff_exptl_absorpt_empirical_full_min 0.930