Cyanide Ligand Assembly by Carbon Atom Transfer to an Iron Nitride.
Martinez, Jorge L.; Lin, Hsiu-Jung; Lee, Wei-Tsung; Pink, Maren; Chen, Chun-Hsing; Gao, Xinfeng; Dickie, Diane A.; Smith, Jeremy M.; Journal of the American Chemical Society  (2017) –; doi:10.1021/jacs.7b08704

data_4126490
_publ_section_title
;
 Cyanide Ligand Assembly by Carbon Atom Transfer to an Iron Nitride.
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.7b08704
_journal_year                    2017
_chemical_formula_moiety         'C49 H78 B Fe N11, 1.50 C4 H8 O'
_chemical_formula_sum            'C55 H90 B Fe N11 O1.5'
_chemical_formula_weight         996.03
_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   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 103.287(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.3404(8)
_cell_length_b                   19.2823(10)
_cell_length_c                   18.4178(10)
_cell_measurement_reflns_used    9826
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.51
_cell_measurement_theta_min      2.51
_cell_volume                     5647.7(5)
_computing_cell_refinement       'APEX II v2014.11-0 (Bruker, 2014)'
_computing_data_collection       'APEX II v2014.11-0 (Bruker, 2014)'
_computing_data_reduction        'APEX II v2014.11-0 (Bruker, 2014)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2013)'
_computing_publication_material  'SHELXTL (Bruker, 2013)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX (Bruker, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Bruker APEXII'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
'0.50 degree frames measured for 10 seconds each'
_diffrn_measurement_device       'APEX Kappa Duo'
_diffrn_measurement_device_type  Kappa
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0428
_diffrn_reflns_av_unetI/netI     0.0403
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            48115
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.580
_diffrn_reflns_theta_min         1.504
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6552
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, G. Sheldrick; 2014'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       block
_exptl_crystal_F_000             2160
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.544
_refine_diff_density_min         -0.448
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     673
_refine_ls_number_reflns         13037
_refine_ls_number_restraints     231
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0574
_refine_ls_R_factor_gt           0.0417
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0435P)^2^+3.0700P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1005
_refine_ls_wR_factor_ref         0.1087
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10352
_reflns_number_total             13037
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b08704_si_002.cif
_cod_data_source_block           15042
_cod_original_formula_sum        'C55 H90 B Fe N11 O1.50'
_cod_database_code               4126490
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.906
_shelx_estimated_absorpt_t_max   0.925
_shelx_res_checksum              86263
_shelx_hkl_checksum              58266