Non-symmetrical, potentially redox non-innocent imino NHC pyridine 'pincers' via a zinc ion template-assisted synthesis.
Simler, Thomas; Danopoulos, Andreas A.; Braunstein, Pierre; Dalton transactions (Cambridge, England : 2003) 46 (2017) 5955–5964; doi:10.1039/c7dt01014a

data_7702131
_publ_section_title
;
 Non-symmetrical, potentially redox non-innocent imino NHC pyridine
 'pincers' via a zinc ion template-assisted synthesis.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5955
_journal_page_last               5964
_journal_paper_doi               10.1039/c7dt01014a
_journal_volume                  46
_journal_year                    2017
_chemical_formula_moiety         'C60 H68 Fe N8'
_chemical_formula_sum            'C60 H68 Fe N8'
_chemical_formula_weight         957.07
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-01-30 deposited with the CCDC.
2017-03-30 downloaded from the CCDC.
;
_cell_angle_alpha                96.111(3)
_cell_angle_beta                 96.654(3)
_cell_angle_gamma                100.812(3)
_cell_formula_units_Z            2
_cell_length_a                   11.2073(14)
_cell_length_b                   13.8988(19)
_cell_length_c                   20.840(3)
_cell_measurement_reflns_used    9905
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.33
_cell_volume                     3139.6(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.0783
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            57104
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.268
_diffrn_reflns_theta_min         1.505
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6218
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.012
_exptl_crystal_description       prism
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.160
_platon_squeeze_details
;
The residual electron density was assigned to two molecules of the diethyl ether solvent [139/2 = 70 e per asymmetric unit; 
two molecules of C4H(10)O1 would give 84 e]. 
;
_refine_diff_density_max         1.978
_refine_diff_density_min         -1.018
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     636
_refine_ls_number_reflns         15358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1314
_refine_ls_R_factor_gt           0.0982
_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^)+(0.0539P)^2^+12.8808P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2210
_refine_ls_wR_factor_ref         0.2331
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10478
_reflns_number_total             15358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01014a2.cif
_cod_data_source_block           pbts150812
_cod_original_cell_volume        3139.7(7)
_cod_database_code               7702131
_shelx_estimated_absorpt_t_min   0.909
_shelx_estimated_absorpt_t_max   0.957
_shelxl_version_number           2013-4
_shelx_res_checksum              32904