5-Ferrocenyl-2,2 -bipyridine Ligands: synthesis, palladium(II) and copper(I) complexes, optical and electrochemical properties.
Crowley, James D.; Scottwell, Synove O.; McAdam, C. John; Shaffer, Karl J.; RSC Advances  (2014) –; doi:10.1039/C4RA05333H

data_7217613
_publ_section_title
;
 5-Ferrocenyl-2,2 -bipyridine Ligands: synthesis, palladium(II) and
 copper(I) complexes, optical and electrochemical properties.
;
_journal_name_full               'RSC Advances'
_journal_paper_doi               10.1039/C4RA05333H
_journal_year                    2014
_chemical_formula_sum            'C49 H46 Cu F6 Fe N4 P'
_chemical_formula_weight         955.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   39.118(3)
_cell_length_b                   39.118(3)
_cell_length_c                   12.8349(11)
_cell_measurement_reflns_used    9837
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      24.354
_cell_measurement_theta_min      2.3285
_cell_volume                     19640(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\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  0.0731
_diffrn_reflns_av_sigmaI/netI    0.0384
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -48
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            136258
_diffrn_reflns_theta_full        26.46
_diffrn_reflns_theta_max         26.46
_diffrn_reflns_theta_min         1.04
_exptl_absorpt_coefficient_mu    0.820
_exptl_absorpt_correction_T_max  0.7195
_exptl_absorpt_correction_T_min  0.5258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.292
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             7872
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.43
_platon_squeeze_details
;
The packing of the crystal shows sizeable solvent channels containing significant 
amounts of diffuse electron density, accounted for by disordered 
solvent which could not be modelled as discrete molecules. As such, PLATON SQUEEZE 
was employed to calculate the contribution to the diffraction from the solvent 
channels and thereby produced a set of solvent-free diffraction intensities. SQUEEZE
estimated four 'voids' containing 220 electrons each. This can be attributed to a 
number of different solvent combinations including water, acetone and various
hydrocarbons originating from petroleum ether.
;
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     566
_refine_ls_number_reflns         10065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.141
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+71.7227P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1331
_reflns_number_gt                8201
_reflns_number_total             10065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra05333h2.cif
_cod_data_source_block           sos072
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_sg_symbol_H-M      I4(1)/a
_cod_database_code               7217613