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_4135003
_publ_section_title
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 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 H77 Cl Fe2 N2 P6'
_chemical_formula_sum            'C55 H77 Cl Fe2 N2 P6'
_chemical_formula_weight         1099.15
_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
_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                 112.32(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   30.198(15)
_cell_length_b                   24.870(8)
_cell_length_c                   20.882(13)
_cell_measurement_reflns_used    1098
_cell_measurement_temperature    100.01
_cell_measurement_theta_max      54.32
_cell_measurement_theta_min      3.16
_cell_volume                     14508(13)
_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)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.907
_diffrn_measured_fraction_theta_max 0.907
_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  0.1959
_diffrn_reflns_av_unetI/netI     0.3224
_diffrn_reflns_Laue_measured_fraction_full 0.907
_diffrn_reflns_Laue_measured_fraction_max 0.907
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19763
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.907
_diffrn_reflns_theta_full        55.214
_diffrn_reflns_theta_max         55.214
_diffrn_reflns_theta_min         2.379
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    5.011
_exptl_absorpt_correction_T_max  0.7508
_exptl_absorpt_correction_T_min  0.4956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1170 before and 0.0888 after correction.
The Ratio of minimum to maximum transmission is 0.6601.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.006
_exptl_crystal_description       plank
_exptl_crystal_F_000             4640
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.061
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.897
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     611
_refine_ls_number_reflns         8347
_refine_ls_number_restraints     750
_refine_ls_restrained_S_all      0.865
_refine_ls_R_factor_all          0.2311
_refine_ls_R_factor_gt           0.1024
_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^)+(0.1049P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2230
_refine_ls_wR_factor_ref         0.2889
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2729
_reflns_number_total             8347
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c01896_si_001.cif
_cod_data_source_block           v19081
_cod_original_cell_volume        14507(13)
_cod_database_code               4135003
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.767
_shelx_estimated_absorpt_t_min   0.483
_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. Restrained distances
 N1-N2
 1.11 with sigma of 0.02
3. Rigid bond restraints
 C48, C47, C49
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C12, Fe1, P1, P2, P3, N1, C1, C3, C6, C11, C18, C21, C17, C27, C24, N2, C2,
 C4, C7, C13, C10, C19, C20, C23, C22, C16, C29, C28, C25, C26, C31, C5, C8,
 C14, C9, C15, P4, C30, Fe2, C32, C38, P5, P6, Cl1, C33, C37, C39, C43, C44,
 C47, C50, C53, C34, C36, C40, C42, C45, C46, C49, C48, C52, C51, C55, C54, C35,
  C41
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
N1 \\sim N2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08 within 1.7A
C47 \\sim C48 \\sim C49: within 1.7A with sigma of 0.04 and sigma for terminal
atoms of 0.08 within 1.7A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Ternary CH refined with riding coordinates:
 C44(H44), C50(H50), C47(H47), C27(H27), C53(H53), C18(H18), C24(H24), C21(H21)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
6.c Aromatic/amide H refined with riding coordinates:
 C13(H13), C33(H33), C30(H30), C14(H14), C4(H4), C36(H36), C7(H7), C16(H16),
 C41(H41), C42(H42), C8(H8), C10(H10), C39(H39), C5(H5), C15(H15), C9(H9),
 C35(H35), C40(H40), C34(H34)
6.d Idealised Me refined as rotating group:
 C55(H55A,H55B,H55C), C49(H49A,H49B,H49C), C26(H26A,H26B,H26C), C19(H19A,H19B,
 H19C), C54(H54A,H54B,H54C), C29(H29A,H29B,H29C), C45(H45A,H45B,H45C), C52(H52A,
 H52B,H52C), C28(H28A,H28B,H28C), C48(H48A,H48B,H48C), C25(H25A,H25B,H25C),
 C46(H46A,H46B,H46C), C20(H20A,H20B,H20C), C51(H51A,H51B,H51C), C23(H23A,H23B,
 H23C), C22(H22A,H22B,H22C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              20020
_shelx_hkl_checksum              79217
_shelx_fab_checksum              10613
_olex2_submission_special_instructions 'No special instructions were received'