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_4135002
_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 Fe2 N4 P6'
_chemical_formula_sum            'C55 H78 Fe2 N4 P6'
_chemical_formula_weight         1092.73
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 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                 108.130(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.123(3)
_cell_length_b                   17.599(3)
_cell_length_c                   18.209(2)
_cell_measurement_reflns_used    9902
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      79.36
_cell_measurement_theta_min      2.51
_cell_volume                     5519.4(15)
_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    'XS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CPAD Area Detector'
_diffrn_detector_area_resol_mean 7.69
_diffrn_detector_type            'Bruker PHOTON II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.960
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0910
_diffrn_reflns_av_unetI/netI     0.0702
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            50951
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.705
_diffrn_reflns_theta_min         3.004
_diffrn_source                   'microfocus sealed tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\mS HB'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.158
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1228 before and 0.0812 after correction.
The Ratio of minimum to maximum transmission is 0.6463.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.315
_exptl_crystal_description       block
_exptl_crystal_F_000             2312
_exptl_crystal_size_max          0.257
_exptl_crystal_size_mid          0.086
_exptl_crystal_size_min          0.079
_refine_diff_density_max         1.166
_refine_diff_density_min         -0.635
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     632
_refine_ls_number_reflns         11649
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0836
_refine_ls_R_factor_gt           0.0633
_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^)+(0.1135P)^2^+0.3246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1696
_refine_ls_wR_factor_ref         0.1868
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8711
_reflns_number_total             11649
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01896_si_001.cif
_cod_data_source_block           v19456
_cod_original_cell_volume        5519.0(15)
_cod_database_code               4135002
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.642
_shelx_estimated_absorpt_t_min   0.301
_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
 Fe2-H3 \\sim Fe2-H2
 with sigma of 0.02
3.a Ternary CH refined with riding coordinates:
 C47(H47), C44(H44), C50(H50), C21(H21), C18(H18), C53(H53), C28(H28), C24(H24)
3.b Aromatic/amide H refined with riding coordinates:
 C40(H40), C35(H35), C30(H30), C8(H8), C14(H14), C36(H36), C34(H34), C7(H7),
 C5(H5), C42(H42), C39(H39), C33(H33), C13(H13), C10(H10), C41(H41), C9(H9),
 C15(H15), C16(H16), C4(H4)
3.c Idealised Me refined as rotating group:
 C52(H52A,H52B,H52C), C55(H55A,H55B,H55C), C45(H45A,H45B,H45C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C), C46(H46A,H46B,H46C), C23(H23A,H23B,H23C), C51(H51A,
 H51B,H51C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C), C54(H54A,H54B,H54C),
 C19(H19A,H19B,H19C), C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C25(H25A,H25B,
 H25C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              27804
_shelx_hkl_checksum              99607
_olex2_submission_special_instructions 'No special instructions were received'