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_4134999
_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 H76 Fe2 P6, 2(C5 H12)'
_chemical_formula_sum            'C65 H100 Fe2 P6'
_chemical_formula_weight         1178.96
_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     direct
_audit_creation_date             2019-12-19
_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                 90.577(15)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.878(4)
_cell_length_b                   16.350(5)
_cell_length_c                   25.612(5)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      79.857
_cell_measurement_theta_min      4.014
_cell_volume                     6230(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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.985
_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  0.0496
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            58255
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.411
_diffrn_reflns_theta_min         3.451
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.469
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.5175
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1087 before and 0.0740 after correction. The Ratio of minimum to maximum transmission is 0.6861. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.301
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.363
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     343
_refine_ls_number_reflns         6723
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0296
_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^)+(0.0368P)^2^+6.7453P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6420
_reflns_number_total             6723
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01896_si_001.cif
_cod_data_source_block           v19171
_cod_database_code               4134999
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.354
_shelx_estimated_absorpt_t_min   0.290
_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 Ternary CH refined with riding coordinates:
 C24(H24), C21(H21), C18(H18), C27(H27)
2.b Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C32(H32A,H32B), C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C7(H7), C15(H15), C5(H5), C16(H16), C9(H9), C13(H13), C8(H8), C10(H10),
 C14(H14), C4(H4)
2.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C28(H28A,H28B,H28C), C26(H26A,H26B,H26C), C29(H29A,H29B,
 H29C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C22(H22A,H22B,H22C), C30(H30A,
 H30B,H30C), C34(H34A,H34B,H34C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              45018
_shelx_hkl_checksum              42337
_olex2_submission_special_instructions 'No special instructions were received'