A Terminal N2 Complex of High-Spin Iron(I) in a Weak, Trigonal Ligand Field.
McSkimming, Alex; Harman, W. Hill; Journal of the American Chemical Society 137 (2015) 8940–8943; doi:10.1021/jacs.5b06337

data_4124417
_publ_section_title
;
 A Terminal N2 Complex of High-Spin Iron(I) in a Weak, Trigonal Ligand
 Field.
;
_journal_issue                   28
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8940
_journal_page_last               8943
_journal_paper_doi               10.1021/jacs.5b06337
_journal_volume                  137
_journal_year                    2015
_chemical_formula_sum            'C56 H74 B Fe N8'
_chemical_formula_weight         925.89
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 92.1689(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.5211(8)
_cell_length_b                   18.3093(13)
_cell_length_c                   23.3063(16)
_cell_measurement_reflns_used    9465
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.24
_cell_measurement_theta_min      2.22
_cell_volume                     4912.8(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_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  0.0432
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            141158
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.508
_diffrn_reflns_theta_min         1.415
_exptl_absorpt_coefficient_mu    0.354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.252
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate frag'
_exptl_crystal_F_000             1988
_exptl_crystal_size_max          0.501
_exptl_crystal_size_mid          0.362
_exptl_crystal_size_min          0.042
_exptl_transmission_factor_max   0.746
_exptl_transmission_factor_min   0.687
_refine_diff_density_max         0.480
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     668
_refine_ls_number_reflns         14975
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0542P)^2^+2.1485P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1138
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11215
_reflns_number_total             14975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b06337_si_002.cif
_cod_data_source_block           hh91AM32_tol_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_database_code               4124417
_shelx_estimated_absorpt_t_min   0.843
_shelx_estimated_absorpt_t_max   0.985
_shelxl_version_number           2013-4
_shelx_res_checksum              76435
_shelx_hkl_checksum              26152