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_2019635
_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)2] [Fe (C10 H8 N2)3] (C14 H10)'
_chemical_formula_moiety
'2(C18 H36 K N2 O6 +), C30 H24 Fe N6 -, C14 H10 -'
_chemical_formula_sum            'C80 H106 Fe K2 N10 O12'
_chemical_formula_weight         1533.79
_chemical_name_common            2249
_chemical_name_systematic
;
Bis[([2.2.2]cryptand)potassium(I)] tris(2,2'-bipyridine)ferrate(--I)
anthrancene(--I)
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_cell_angle_alpha                90
_cell_angle_beta                 109.779(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.049(4)
_cell_length_b                   17.067(3)
_cell_length_c                   21.543(3)
_cell_measurement_reflns_used    2362
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.98
_cell_measurement_theta_min      2.24
_cell_volume                     7975(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.997
_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  0.0849
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22943
_diffrn_reflns_theta_full        25.030
_diffrn_reflns_theta_max         25.081
_diffrn_reflns_theta_min         1.518
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6374
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2012)'
_exptl_crystal_colour            purple--black
_exptl_crystal_density_diffrn    1.277
_exptl_crystal_description       plate
_exptl_crystal_F_000             3264
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.386
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         7069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.1135
_refine_ls_R_factor_gt           0.0569
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0515P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1039
_refine_ls_wR_factor_ref         0.1219
_reflns_number_gt                4398
_reflns_number_total             7069
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ov3050sup1.cif
_cod_data_source_block           1
_cod_database_code               2019635
_cod_database_fobs_code          2019635
_shelx_estimated_absorpt_t_min   0.864
_shelx_estimated_absorpt_t_max   0.979
_shelx_hkl_checksum              32183
_shelx_res_checksum              45978
_shelxl_version_number           2.014