Mimicking the Constrained Geometry of a Nitrogen-Fixation Intermediate.
Liu, Tianchang; Gau, Michael R.; Tomson, Neil C.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c01861

data_4134759
_publ_section_title
;
 Mimicking the Constrained Geometry of a Nitrogen-Fixation Intermediate.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c01861
_journal_year                    2020
_chemical_formula_moiety         'C68 H76 Fe2 N8 P2, 2(C4 H10 O)'
_chemical_formula_sum            'C76 H96 Fe2 N8 O2 P2'
_chemical_formula_weight         1327.24
_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_creation_date             2019-12-16
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                91.674(2)
_cell_angle_beta                 98.0110(10)
_cell_angle_gamma                98.486(2)
_cell_formula_units_Z            2
_cell_length_a                   10.6831(2)
_cell_length_b                   16.4143(4)
_cell_length_c                   20.2856(4)
_cell_measurement_reflns_used    34365
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.5480
_cell_measurement_theta_min      2.4040
_cell_volume                     3479.41(13)
_computing_cell_refinement       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.61a (Rigaku OD, 2019)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 2012)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100
_diffrn_detector                 'HPC area detector'
_diffrn_detector_area_resol_mean 10.0
_diffrn_detector_type            'Dectris PILATUS3 R 200K'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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    -21.00  97.00   0.50   30.00    --   15.97  54.00-102.00  236
  2  \w     41.00  99.00   0.50   30.00    --   15.97 178.00 120.00  116
  3  \w     41.00  99.00   0.50   30.00    --   15.97 178.00 150.00  116
  4  \w    -24.00  99.00   0.50   30.00    --   15.97  77.00   0.00  246
  5  \w    -23.00  66.00   0.50   30.00    --   15.97 -99.00   0.00  178
  6  \w    -23.00  34.00   0.50   30.00    --  -16.36 -99.00  90.00  114
  7  \w    -23.00  66.00   0.50   30.00    --   15.97 -99.00 120.00  178
  8  \w    -23.00  34.00   0.50   30.00    --  -16.36 -99.00   0.00  114
  9  \w    -23.00  34.00   0.50   30.00    --  -16.36 -99.00 -90.00  114
 10  \w    -65.00  40.00   0.50   30.00    --   15.97 -54.00 113.00  210
 11  \w    -52.00  65.00   0.50   30.00    --  -16.36  54.00-102.00  234
 12  \w    -52.00  64.00   0.50   30.00    --  -16.36  57.00 -60.00  232
 13  \w    -70.00  21.00   0.50   30.00    --   15.97 -37.00 150.00  182
 14  \w    -74.00   5.00   0.50   30.00    --   15.97 -19.00  30.00  158
 15  \w    -97.00  19.00   0.50   30.00    --  -16.36 -54.00 113.00  232
 16  \w   -106.00 -71.00   0.50   30.00    --  -16.36 -19.00-180.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku XtaLAB Synergy-S'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0084181000
_diffrn_orient_matrix_UB_12      -0.0350786000
_diffrn_orient_matrix_UB_13      0.0194460000
_diffrn_orient_matrix_UB_21      -0.0672233000
_diffrn_orient_matrix_UB_22      -0.0009301000
_diffrn_orient_matrix_UB_23      -0.0060258000
_diffrn_orient_matrix_UB_31      -0.0037096000
_diffrn_orient_matrix_UB_32      -0.0261238000
_diffrn_orient_matrix_UB_33      -0.0289064000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.070
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            127175
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.571
_diffrn_reflns_theta_min         2.030
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet-S (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.515
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74736
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       bar
_exptl_crystal_F_000             1412
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.866
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     826
_refine_ls_number_reflns         26672
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0557
_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^)+(0.0806P)^2^+3.9342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1501
_reflns_number_gt                22681
_reflns_number_total             26672
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by -179.9160\% 
 around [0.00 0.71 -0.70] (reciprocal) or [0.05 0.84 -0.53] (direct)
;
_cod_data_source_file            ja0c01861_si_003.cif
_cod_data_source_block           3723
_cod_database_code               4134759
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5613(8)
 0.4387(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B), C10(H10A,H10B), C18(H18A,H18B), C19(H19A,H19B),
 C20(H20A,H20B), C70(H70A,H70B), C71(H71A,H71B), C74(H74A,H74B), C75(H75A,H75B)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C13(H13), C15(H15), C34(H34), C35(H35), C36(H36), C37(H37),
 C38(H38), C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C46(H46), C47(H47),
  C48(H48), C49(H49), C50(H50), C52(H52), C53(H53), C54(H54), C55(H55),
 C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62), C64(H64), C65(H65),
  C66(H66), C67(H67), C68(H68)
3.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A,H24B,H24C), C25(H25A,H25B,
 H25C), C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C29(H29A,H29B,H29C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C69(H69A,H69B,H69C),
 C72(H72A,H72B,H72C), C73(H73A,H73B,H73C), C76(H76A,H76B,H76C)
;
_shelx_res_checksum              40015
_shelx_hkl_checksum              2190
_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 1.799
_oxdiff_exptl_absorpt_empirical_full_min 0.577
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2