Ferrocenylated Chalcogen (Se and Te)-containing N-heterocyclic carbenes: Selenones, silver and palladium complexes
Gonzalez, Rodary; Azpiroz, Ramón; Sharma, Pankaj; Villamizar C, Claudia P.; Anzaldo, Bertin; Pérez-Flores, Francisco J.; Toscano, Ruben Alfredo; Inorganica Chimica Acta 506 (2020) 119531–; doi:10.1016/j.ica.2020.119531

data_1564970
_publ_section_title
;
 Ferrocenylated Chalcogen (Se and Te)-containing N-heterocyclic carbenes:
 Selenones, silver and palladium complexes
;
_journal_name_full               'Inorganica Chimica Acta'
_journal_page_first              119531
_journal_paper_doi               10.1016/j.ica.2020.119531
_journal_volume                  506
_journal_year                    2020
_chemical_formula_moiety         'C22 H22 Fe N2 Se2'
_chemical_formula_sum            'C22 H22 Fe N2 Se2'
_chemical_formula_weight         528.18
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 97.3480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0188(6)
_cell_length_b                   10.0612(4)
_cell_length_c                   14.3661(5)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.36
_cell_measurement_theta_min      2.48
_cell_volume                     2009.64(14)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      150.01
_diffrn_detector_area_resol_mean 52.0833
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Bruker D8 Venture \k-geometry diffractometer 208039-01'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  'Helios multilayer mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0243
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19894
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.364
_diffrn_reflns_theta_min         2.478
_exptl_absorpt_coefficient_mu    4.382
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.4164
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0978 before and 0.0474 after correction.
The Ratio of minimum to maximum transmission is 0.5588.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            bronze
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1048
_exptl_crystal_size_max          0.377
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.286
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.063
_refine_ls_extinction_coef       .
_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     244
_refine_ls_number_reflns         3680
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0228
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0158P)^2^+1.9052P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0480
_refine_ls_wR_factor_ref         0.0497
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3339
_reflns_number_total             3680
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            354SHP19.cif
_cod_data_source_block           354shp19
_cod_database_code               1564970
_shelx_estimated_absorpt_t_max   0.367
_shelx_estimated_absorpt_t_min   0.289
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C15(H15A,H15B), C16(H16A,H16B)
2.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C3(H3), C5(H5), C7(H7), C6(H6), C8(H8), C9(H9), C10(H10),
 C13(H13), C14(H14), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
;
_shelx_res_checksum              92261
_shelx_hkl_checksum              70202
_olex2_submission_special_instructions 'No special instructions were received'