Synthesis and structural characterization of electrochemically reversible bisferrocenes containing bis(acyl-thiourea)s: enantiomers and conformers
Duan, Xin-E; Li, Rui; Tong, Hong-Bo; Li, Ying-Qi; Bai, Sheng-Di; Guo, Yu-Jing; Liu, Dian-Sheng; New J. Chem. 41 (2017) 3333–; doi:10.1039/C6NJ03539F

data_1545616
_publ_section_title
;
 Synthesis and structural characterization of electrochemically reversible
 bisferrocenes containing bis(acyl-thiourea)s: enantiomers and conformers
;
_journal_issue                   9
_journal_name_full               'New J. Chem.'
_journal_page_first              3333
_journal_paper_doi               10.1039/C6NJ03539F
_journal_volume                  41
_journal_year                    2017
_chemical_absolute_configuration syn
_chemical_formula_sum            'C42 H44 Fe2 N4 O2 S2'
_chemical_formula_weight         812.63
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-15 deposited with the CCDC.
2017-03-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.615(6)
_cell_length_b                   9.703(7)
_cell_length_c                   52.00(3)
_cell_measurement_reflns_used    8294
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.15
_cell_measurement_theta_min      2.24
_cell_volume                     3842(5)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0315
_diffrn_reflns_av_unetI/netI     0.0425
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       54
_diffrn_reflns_limit_l_min       -64
_diffrn_reflns_number            23350
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.996
_diffrn_reflns_theta_min         0.783
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.906
_exptl_crystal_colour            Orange-red
_exptl_crystal_density_diffrn    1.405
_exptl_crystal_description       Needle
_exptl_crystal_F_000             1696
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.320
_exptl_crystal_size_min          0.310
_refine_diff_density_max         0.598
_refine_diff_density_min         -0.586
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.05(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     449
_refine_ls_number_reflns         7538
_refine_ls_number_restraints     246
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0632
_refine_ls_R_factor_gt           0.0580
_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^)+(0.0409P)^2^+7.6149P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1338
_refine_ls_wR_factor_ref         0.1370
_reflns_Friedel_coverage         0.743
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                6963
_reflns_number_total             7538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj03539f2.cif
_cod_data_source_block           S992B
_cod_depositor_comments
'Adding full bibliography for 1545616--1545618.cif.'
_cod_database_code               1545616
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.742
_shelx_estimated_absorpt_t_max   0.767
_shelx_res_checksum              93709