New Multi-Ferrocenyl- and Multi-Ferricenyl- Materials via Coordination-Driven Self-Assembly and via Charge-Driven Electro-Crystallization
Hakikulla H. Shah; Rayya A. Al-Balushi; Mohammed K. Al-Suti; Muhammad S. Khan; Christopher H. Woodall; Anna L. Sudlow; Paul R. Raithby; Gabriele Kociok-Köhn; Kieran C. Molloy; Frank Marken; Inorganic Chemistry 52 (2013) 12012–12022; doi:10.1021/ic401803p

data_4336449
_publ_section_title
;
 New Multi-Ferrocenyl- and Multi-Ferricenyl- Materials via
 Coordination-Driven Self-Assembly and via Charge-Driven
 Electro-Crystallization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12012
_journal_page_last               12022
_journal_paper_doi               10.1021/ic401803p
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C68 H52 Br2 Cu2 Fe4 N4, 0.15(C2 H4 Cl4)'
_chemical_formula_sum            'C68.3 H52.6 Br2 Cl0.6 Cu2 Fe4 N4'
_chemical_formula_weight         1460.91
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.1580(10)
_cell_angle_beta                 92.7480(10)
_cell_angle_gamma                94.4840(10)
_cell_formula_units_Z            2
_cell_length_a                   9.8408(2)
_cell_length_b                   13.3736(3)
_cell_length_c                   23.7742(5)
_cell_measurement_reflns_used    46009
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      2.910
_cell_volume                     3003.14(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
;
 DENZO-SCALEPACK Z. Otwinowski and W. Minor, " 
 Processing of x-ray Diffraction Data Collected in Oscillation Mode ", 
 Methods in Enzymology, Volume 276: Macromolecular Crystallography, 
 part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press.
;
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. H\"ubschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_structure_solution
; 
 SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , 
 Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. 
 (1999) J. Appl. Cryst. 32, 115-119
;
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       '284 2.0 degree images with \f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_av_sigmaI/netI    0.0482
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            40103
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.038
_exptl_absorpt_correction_T_max  0.8629
_exptl_absorpt_correction_T_min  0.4626
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
Sortav (Blessing 1995)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.616
_exptl_crystal_description       plate
_exptl_crystal_F_000             1465
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         5.000
_refine_diff_density_min         -1.936
_refine_diff_density_rms         0.274
_refine_ls_extinction_coef       0.0058(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     750
_refine_ls_number_reflns         10242
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0953
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1779P)^2^+47.6729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2737
_refine_ls_wR_factor_ref         0.2938
_reflns_number_gt                8417
_reflns_number_total             10242
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401803p_si_001_3.cif
_cod_data_source_block           k12kcm46
_cod_original_cell_volume        3003.13(11)
_cod_original_formula_sum        'C68.30 H52.60 Br2 Cl0.60 Cu2 Fe4 N4'
_cod_database_code               4336449