Transition metal mediated formation of dicationic diselenides stabilised by N-heterocyclic carbenes: designed synthesis.
Yadav, Sangeeta; Manjare, Sudesh T.; Singh, Harkesh B.; Butcher, Ray J.; Dalton transactions (Cambridge, England : 2003) 45 (2016) 12015–12027; doi:10.1039/c6dt01425a

data_7039650
_publ_section_title
;
 Transition metal mediated formation of dicationic diselenides stabilised
 by N-heterocyclic carbenes: designed synthesis.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12015
_journal_page_last               12027
_journal_paper_doi               10.1039/c6dt01425a
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
;
2(C30 H44 N4 Se2), 3(Cl4 Fe), Cl
;
_chemical_formula_sum            'C60 H88 Cl13 Fe3 N8 Se4'
_chemical_formula_weight         1865.62
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2016-06-18 deposited with the CCDC.
2016-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.9814(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   29.6082(4)
_cell_length_b                   14.9144(2)
_cell_length_c                   18.6317(3)
_cell_measurement_reflns_used    23868
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      35.0533
_cell_measurement_theta_min      3.0527
_cell_volume                     8222.6(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.5081
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0520
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -47
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            121574
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         35.132
_diffrn_reflns_theta_min         3.060
_exptl_absorpt_coefficient_mu    2.755
_exptl_absorpt_correction_T_max  0.656
_exptl_absorpt_correction_T_min  0.319
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.507
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thick needle'
_exptl_crystal_F_000             3756
_exptl_crystal_size_max          0.5873
_exptl_crystal_size_mid          0.3343
_exptl_crystal_size_min          0.1694
_refine_diff_density_max         1.835
_refine_diff_density_min         -0.802
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     857
_refine_ls_number_reflns         34275
_refine_ls_number_restraints     1215
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.1124
_refine_ls_R_factor_gt           0.0542
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0212P)^2^+11.7389P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0878
_refine_ls_wR_factor_ref         0.1052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19995
_reflns_number_total             34275
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt01425a2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7039650--7039655.cif.'
_cod_database_code               7039650
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              21825