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_1545618
_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_moiety         'C30 H32 Fe2 N4 O2 S2'
_chemical_formula_sum            'C30 H32 Fe2 N4 O2 S2'
_chemical_formula_weight         656.41
_chemical_melting_point          462.0(10)
_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                   9.7134(8)
_cell_length_b                   14.5357(12)
_cell_length_c                   20.8935(17)
_cell_measurement_reflns_used    5092
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      19.94
_cell_measurement_theta_min      2.31
_cell_volume                     2950.0(4)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0647
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            31790
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.050
_diffrn_reflns_theta_max         25.050
_diffrn_reflns_theta_min         1.707
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.160
_exptl_crystal_colour            Orange-red
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_description       Block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.228
_refine_diff_density_min         -0.261
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 1630 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         5232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0331
_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^)+(0.0218P)^2^+0.5910P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0592
_refine_ls_wR_factor_ref         0.0647
_reflns_Friedel_coverage         0.766
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                4340
_reflns_number_total             5232
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6nj03539f2.cif
_cod_data_source_block           s376b
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '461-463' was changed to '462.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 1545616--1545618.cif.
;
_cod_database_code               1545618
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.722
_shelx_estimated_absorpt_t_max   0.801
_shelx_res_checksum              61556