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_4134998
_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 H78 Br2 Fe2 P6'
_chemical_formula_sum            'C55 H78 Br2 Fe2 P6'
_chemical_formula_weight         1196.51
_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   geom
_atom_sites_solution_primary     direct
_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                 93.410(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.847(10)
_cell_length_b                   11.095(2)
_cell_length_c                   16.608(4)
_cell_measurement_reflns_used    9893
_cell_measurement_temperature    99.99
_cell_measurement_theta_max      75.04
_cell_measurement_theta_min      2.80
_cell_volume                     5858(3)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 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    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.99
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1228
_diffrn_reflns_av_unetI/netI     0.0826
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.910
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41187
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.910
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.171
_diffrn_reflns_theta_min         2.780
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    7.366
_exptl_absorpt_correction_T_max  0.7833
_exptl_absorpt_correction_T_min  0.4561
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1608 before and 0.1195 after correction.
The Ratio of minimum to maximum transmission is 0.5823.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_description       plate
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.167
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.174
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     303
_refine_ls_number_reflns         5568
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.2344
_refine_ls_R_factor_gt           0.1879
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+387.4447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3848
_refine_ls_wR_factor_ref         0.4118
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3722
_reflns_number_total             5568
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01896_si_001.cif
_cod_data_source_block           v19222
_cod_database_code               4134998
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.930
_shelx_estimated_absorpt_t_min   0.351
_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. Rigid bond restraints
 C22, C21, C23
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C22 \\sim C21 \\sim C23: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
4. Rigid body (RIGU) restrains
 C22, C21, C23
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H1A(0.5) H1B(0.5) H1C(0.5)
6.a Ternary CH refined with riding coordinates:
 C27(H27), C24(H24), C18(H18), C21(H21)
6.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C7(H7), C8(H8), C10(H10), C9(H9), C13(H13), C14(H14),
 C15(H15), C16(H16)
6.c Idealised Me refined with riding coordinates:
 C1(H1A,H1B,H1C)
6.d Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C26(H26A,H26B,
 H26C), C20(H20A,H20B,H20C), C25(H25A,H25B,H25C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C)
;
_shelx_res_checksum              35944
_shelx_hkl_checksum              43955
_olex2_submission_special_instructions 'No special instructions were received'