Activation of an Open Shell, Carbyne-Bridged Diiron Complex Toward Binding of Dinitrogen.
Arnett, Charles H.; Agapie, Theodor; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c01896

data_4135000
_publ_section_title
;
 Activation of an Open Shell, Carbyne-Bridged Diiron Complex Toward
 Binding of Dinitrogen.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c01896
_journal_year                    2020
_chemical_formula_moiety         'C55 H80 Fe2 N4 P6'
_chemical_formula_sum            'C55 H80 Fe2 N4 P6'
_chemical_formula_weight         1094.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-12-21
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.19(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.05(2)
_cell_length_b                   11.137(11)
_cell_length_c                   16.323(12)
_cell_measurement_reflns_used    6300
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      32.61
_cell_measurement_theta_min      2.27
_cell_volume                     5811(8)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'XT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.836
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.836
_diffrn_reflns_limit_h_max       47
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            66591
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.836
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.317
_diffrn_reflns_theta_min         1.936
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.702
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.9042
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0656 before and 0.0545 after correction.
The Ratio of minimum to maximum transmission is 0.9042.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.251
_exptl_crystal_description       block
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.344
_exptl_crystal_size_mid          0.168
_exptl_crystal_size_min          0.146
_refine_diff_density_max         2.950
_refine_diff_density_min         -1.601
_refine_diff_density_rms         0.109
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         9410
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      1.101
_refine_ls_R_factor_all          0.1020
_refine_ls_R_factor_gt           0.0801
_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^)+(0.0608P)^2^+43.6874P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1846
_refine_ls_wR_factor_ref         0.1970
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7496
_reflns_number_total             9410
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01896_si_001.cif
_cod_data_source_block           d19156
_cod_database_code               4135000
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.904
_shelx_estimated_absorpt_t_min   0.794
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Fe1-H = Fe1-HA
 1.54 with sigma of 0.02
 C19-C18 \\sim C21-C18 \\sim C20-C18 \\sim C24-C22 \\sim C23-C22 \\sim C27-C25
\\sim C26-C25 \\sim C29-C28
 \\sim C30-C28
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C19 \\sim C21 \\sim C20: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
4. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5) C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5)
 C21(0.5) H21A(0.5) H21B(0.5) H21C(0.5)
5.a Ternary CH refined with riding coordinates:
 C28(H28), C25(H25), C22(H22)
5.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C14(H14), C13(H13), C16(H16), C15(H15), C7(H7), C8(H8),
 C10(H10), C9(H9)
5.c Idealised Me refined with riding coordinates:
 C1(H1A,H1B,H1C)
5.d Idealised Me refined as rotating group:
 C29(H29A,H29B,H29C), C30(H30A,H30B,H30C), C27(H27A,H27B,H27C), C26(H26A,H26B,
 H26C), C19(H19A,H19C,H19B), C23(H23A,H23B,H23C), C20(H20A,H20B,H20C), C24(H24A,
 H24B,H24C), C21(H21A,H21B,H21C)
;
_shelx_res_checksum              84996
_shelx_hkl_checksum              71478
_olex2_submission_special_instructions 'No special instructions were received'