Heteroleptic, two-coordinate [M(NHC){N(SiMe3)2}] (M = Co, Fe) complexes: synthesis, reactivity and magnetism rationalized by an unexpected metal oxidation state.
Danopoulos, Andreas A.; Braunstein, Pierre; Monakhov, Kirill Yu; van Leusen, Jan; Kögerler, Paul; Clémancey, Martin; Latour, Jean-Marc; Benayad, Anass; Tromp, Moniek; Rezabal, Elixabete; Frison, Gilles; Dalton transactions (Cambridge, England : 2003) 46 (2017) 1163–1171; doi:10.1039/c6dt03565e

data_7041524
_publ_section_title
;
 Heteroleptic, two-coordinate [M(NHC){N(SiMe3)2}] (M = Co, Fe) complexes:
 synthesis, reactivity and magnetism rationalized by an unexpected metal
 oxidation state.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1163
_journal_page_last               1171
_journal_paper_doi               10.1039/c6dt03565e
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C72 H96 Co2 N6'
_chemical_formula_sum            'C72 H96 Co2 N6'
_chemical_formula_weight         1163.40
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2016-03-17 deposited with the CCDC.
2016-12-21 downloaded from the CCDC.
;
_cell_angle_alpha                102.2490(10)
_cell_angle_beta                 113.9150(10)
_cell_angle_gamma                99.5290(10)
_cell_formula_units_Z            1
_cell_length_a                   12.1174(5)
_cell_length_b                   12.5086(5)
_cell_length_c                   13.6791(5)
_cell_measurement_reflns_used    9341
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.57
_cell_volume                     1777.26(12)
_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-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0257
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            38385
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.024
_diffrn_reflns_theta_min         1.713
_diffrn_source                   'fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.508
_exptl_absorpt_correction_T_max  0.7460
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_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
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_exptl_crystal_density_diffrn    1.087
_exptl_crystal_description       block
_exptl_crystal_F_000             624
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_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_platon_squeeze_details
;
 The residual electron density was assigned to half a molecule of the
 pentane solvent [55/2 = 28 e per asymmetric unit; half a molecule of
 C5H12 would give 21e].
;
_refine_diff_density_max         1.455
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         10340
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0835P)^2^+0.1635P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1300
_refine_ls_wR_factor_ref         0.1359
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8633
_reflns_number_total             10340
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03565e2.cif
_cod_data_source_block           pbad150623
_cod_depositor_comments
'Adding full bibliography for 7041522--7041525.cif.'
_cod_database_code               7041524
_shelx_estimated_absorpt_t_min   0.842
_shelx_estimated_absorpt_t_max   0.905
_shelxl_version_number           2013-4
_shelx_res_checksum              50333