Structural, Electronic, and Computational Studies of Heteroleptic Cu(I) Complexes of 6,6'-Dimesityl-2,2'-bipyridine with Ferrocene-Appended Ethynyl-2,2'-bipyridine Ligands.
Barnsley, Jonathan E.; Scottwell, Synøve Ø; Elliott, Anastasia B. S.; Gordon, Keith C.; Crowley, James D.; Inorganic chemistry 55 (2016) 8184–8192; doi:10.1021/acs.inorgchem.6b01300

data_4348527
_publ_section_title
;
 Structural, Electronic, and Computational Studies of Heteroleptic Cu(I)
 Complexes of 6,6'-Dimesityl-2,2'-bipyridine with Ferrocene-Appended
 Ethynyl-2,2'-bipyridine Ligands.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8184
_journal_page_last               8192
_journal_paper_doi               10.1021/acs.inorgchem.6b01300
_journal_volume                  55
_journal_year                    2016
_chemical_formula_sum            'C56 H56 Cu F6 Fe N4 O2 P'
_chemical_formula_weight         1081.42
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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                71.505(6)
_cell_angle_beta                 76.440(6)
_cell_angle_gamma                78.322(7)
_cell_formula_units_Z            2
_cell_length_a                   10.9313(14)
_cell_length_b                   14.207(2)
_cell_length_c                   19.792(3)
_cell_measurement_reflns_used    8893
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.9895
_cell_measurement_theta_min      2.2075
_cell_volume                     2806.2(7)
_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, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.962
_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  0.0622
_diffrn_reflns_av_sigmaI/netI    0.0763
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_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            37710
_diffrn_reflns_theta_full        26.74
_diffrn_reflns_theta_max         26.74
_diffrn_reflns_theta_min         1.10
_exptl_absorpt_coefficient_mu    0.728
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.79
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
Although two acetone molecules could be assigned per asymmetric unit, there
remained diffuse electron density within the solvent accessible void, accounted
for by disordered solvent which could not be modelled sensibly as discrete 
molecules. As such, PLATON SQUEEZE was employed to calculate the contribution to 
the diffraction from the solvent void and thereby produced a set of solvent-free
diffraction intensities. SQUEEZE estimated a single void containing 23.5 electrons
per unit cell. The void sits on the face of the cell, thus there is a 23.5 electron
contribution from two separate unit cells, giving a total void electron count of 
47. This can be accounted for by one acetone molecule and one and a half water 
molecules disordered between the two adjacent unit cells.
;
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.564
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         11469
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0623
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1079P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1685
_refine_ls_wR_factor_ref         0.1849
_reflns_number_gt                7734
_reflns_number_total             11469
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01300_si_002.cif
_cod_data_source_block           dp002_1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        2806.3(7)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4348527