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_7702130
_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, Br'
_chemical_formula_sum            'C60 H68 Br Fe N8'
_chemical_formula_weight         1036.98
_space_group_crystal_system      orthorhombic
_space_group_IT_number           41
_space_group_name_Hall           'A 2 -2ab'
_space_group_name_H-M_alt        'A e a 2'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.9792(10)
_cell_length_b                   29.3525(12)
_cell_length_c                   18.8532(8)
_cell_measurement_reflns_used    7345
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.73
_cell_measurement_theta_min      2.49
_cell_volume                     13269.8(10)
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0820
_diffrn_reflns_av_unetI/netI     0.1107
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            55451
_diffrn_reflns_point_group_measured_fraction_full 0.923
_diffrn_reflns_point_group_measured_fraction_max 0.883
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.029
_diffrn_reflns_theta_min         1.387
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6675
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.038
_exptl_crystal_description       prism
_exptl_crystal_F_000             4360
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.120
_platon_squeeze_details
;
The residual electron density was assigned to two and a half a molecule of 
tetrahydrofuran solvent [819/8= 102 e per asymmetric unit; 
two and a half a molecule of C4 H8 O1 would give 100 e].
;
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.051
_refine_ls_abs_structure_details
;
 Flack x determined using 3170 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.002(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         17156
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.1040
_refine_ls_R_factor_gt           0.0497
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0292P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.0908
_reflns_Friedel_coverage         0.719
_reflns_Friedel_fraction_full    0.841
_reflns_Friedel_fraction_max     0.761
_reflns_number_gt                9672
_reflns_number_total             17156
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt01014a2.cif
_cod_data_source_block           pbts160609
_cod_original_sg_symbol_Hall     'A 2 -2ac'
_cod_original_sg_symbol_H-M      'A b a 2'
_cod_database_code               7702130
_shelx_estimated_absorpt_t_min   0.751
_shelx_estimated_absorpt_t_max   0.903
_shelxl_version_number           2013-4
_shelx_res_checksum              21085