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_4348528
_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            'C62 H52 Cu F6 Fe2 N4 O0 P'
_chemical_formula_weight         1173.29
_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                95.364(5)
_cell_angle_beta                 92.364(4)
_cell_angle_gamma                114.839(4)
_cell_formula_units_Z            4
_cell_length_a                   14.1641(11)
_cell_length_b                   15.7908(11)
_cell_length_c                   29.130(2)
_cell_measurement_reflns_used    6184
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.884
_cell_measurement_theta_min      2.531
_cell_volume                     5863.3(8)
_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 0.988
_diffrn_measured_fraction_theta_max 0.988
_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  0.1136
_diffrn_reflns_av_sigmaI/netI    0.1342
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            122186
_diffrn_reflns_theta_full        26.52
_diffrn_reflns_theta_max         26.52
_diffrn_reflns_theta_min         0.70
_exptl_absorpt_coefficient_mu    0.935
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6923
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2009)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2408
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
Although attempts were made to model discrete solvent molecules, there
remained diffuse electron density within the solvent accessible void, accounted
for by disordered solvent which could not be modelled sensibly. 
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 195 electrons
per unit cell. This can be accounted for by a number of combinations, including
five molecules of acetone and three and a half molecules of water, or three
molecules of diethyl ether, two of acetone, and half a molecule of water.

;
_refine_diff_density_max         1.813
_refine_diff_density_min         -1.711
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1377
_refine_ls_number_reflns         24061
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.1697
_refine_ls_R_factor_gt           0.0952
_refine_ls_shift/su_max          0.058
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1580P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2556
_refine_ls_wR_factor_ref         0.2896
_reflns_number_gt                11262
_reflns_number_total             24061
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b01300_si_002.cif
_cod_data_source_block           sos090_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_sg_symbol_H-M      P-1
_cod_database_code               4348528