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_4134760
_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         'C38 H64 Fe2 N8 P2, C4 H10 O, 0.5(C6 H14)'
_chemical_formula_sum            'C45 H81 Fe2 N8 O P2'
_chemical_formula_weight         923.81
_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             2019-11-13
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                91.874(2)
_cell_angle_beta                 92.340(2)
_cell_angle_gamma                106.816(2)
_cell_formula_units_Z            2
_cell_length_a                   9.8631(6)
_cell_length_b                   13.0959(8)
_cell_length_c                   20.1607(12)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.533
_cell_measurement_theta_min      2.885
_cell_volume                     2487.9(3)
_computing_cell_refinement       'SAINT V8.38A (2016)'
_computing_data_collection       'Bruker APEX3 v2018.7-2'
_computing_data_reduction        'SAINT V8.38A (2016)'
_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_temperature      100
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'CMOS area detector'
_diffrn_measurement_device_type  'Bruker D8QUEST'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0404
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            52187
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.548
_diffrn_reflns_theta_min         2.524
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.688
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014/5'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.233
_exptl_crystal_description       irregular
_exptl_crystal_F_000             994
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.534
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     542
_refine_ls_number_reflns         11406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0603
_refine_ls_R_factor_gt           0.0440
_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^)+(0.0215P)^2^+5.3200P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1063
_reflns_number_gt                9330
_reflns_number_total             11406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01861_si_002.cif
_cod_data_source_block           3716
_cod_database_code               4134760
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. 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
2.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), C40(H40A,H40B), C41(H41A,H41B), C43(H43A,H43B), C44(H44A,H44B)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C13(H13), C15(H15)
2.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), C33(H33A,H33B,H33C),
 C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C37(H37A,H37B,
 H37C), C38(H38A,H38B,H38C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C45(H45A,
 H45B,H45C)
;
_shelx_res_checksum              26112
_shelx_hkl_checksum              33256
_olex2_submission_special_instructions 'No special instructions were received'