Homoleptic 2,2'-bipyridine metalates(‒I) of iron and cobalt, one cocrystallized with an anthracene radical anion and the other with neutral anthracene
Brennessel, William W.; Ellis, John E.; Acta Crystallographica Section C 70 (2014) 828–832; doi:10.1107/S2053229614017070

data_2019636
_publ_section_title
;
 Homoleptic 2,2'-bipyridine metalates(--I) of iron and cobalt, one
 cocrystallized with an anthracene radical anion and the other with
 neutral anthracene
;
_journal_coeditor_code           OV3050
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              828
_journal_page_last               832
_journal_paper_doi               10.1107/S2053229614017070
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac
'[K (C18 H36 N2 O6)] [Co (C10 H8 N2)2], 0.5C14 H10, 2C4 H8 O'
_chemical_formula_moiety
'C18 H36 K N2 O6 +, C20 H16 Co N4 -, 0.5(C14 H10), 2(C4 H8 O)'
_chemical_formula_sum            'C53 H73 Co K N6 O8'
_chemical_formula_weight         1020.20
_chemical_name_common            2225
_chemical_name_systematic
;
([2.2.2]Cryptand)potassium(I) bis(2,2'-bipyridine)cobaltate(--I) anthrancene
hemisolvate tetrahydrofuran disolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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-2014
_cell_angle_alpha                99.1054(13)
_cell_angle_beta                 90.8279(14)
_cell_angle_gamma                109.2433(13)
_cell_formula_units_Z            2
_cell_length_a                   10.5981(8)
_cell_length_b                   14.4323(11)
_cell_length_c                   18.4886(15)
_cell_measurement_reflns_used    3379
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.32
_cell_volume                     2629.5(4)
_computing_cell_refinement       'SAINT (Bruker, 2003)'
_computing_data_collection       'SMART (Bruker, 2003)'
_computing_data_reduction        'SAINT (Bruker, 2003)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL2014 (Sheldrick, 2014)'
_computing_structure_solution    'SIR97 (Altomare <i>et al.</i>, 1999)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Siemens SMART CCD platform'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0212
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26404
_diffrn_reflns_theta_full        25.028
_diffrn_reflns_theta_max         25.031
_diffrn_reflns_theta_min         1.118
_exptl_absorpt_coefficient_mu    0.463
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2012)'
_exptl_crystal_colour            purple-black
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       rod
_exptl_crystal_F_000             1086
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.312
_refine_diff_density_min         -0.221
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         9299
_refine_ls_number_restraints     257
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0433
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0385P)^2^+0.7396P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                7616
_reflns_number_total             9299
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ov3050sup1.cif
_cod_data_source_block           2
_cod_database_code               2019636
_cod_database_fobs_code          2019636
_shelx_estimated_absorpt_t_min   0.836
_shelx_estimated_absorpt_t_max   0.946
_shelx_hkl_checksum              54320
_shelx_res_checksum              65247
_shelxl_version_number           2.014