Crystal structure of {2,2'-[<i>N</i>,<i>N</i>'-bis(pyridin-2-ylmethyl)cyclohexane-<i>trans</i>-1,2-diyldi(nitrilo)]diacetato}cobalt(III) hexafluoridophosphate
McLauchlan, Craig C.; Kissel, Daniel S.; Herlinger, Albert W.; Acta Crystallographica Section E 71 (2015) 380–384; doi:10.1107/S2056989015005149

data_2240516
_publ_section_title
;
 Crystal structure of
 {2,2'-[<i>N</i>,<i>N</i>'-bis(pyridin-2-ylmethyl)cyclohexane-<i>trans</i>-1,2-diyldi(nitrilo)]diacetato}cobalt(III)
 hexafluoridophosphate
;
_journal_coeditor_code           ZL2616
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              380
_journal_page_last               384
_journal_paper_doi               10.1107/S2056989015005149
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Co (C22 H26 N4 O4)] P F6'
_chemical_formula_moiety         'C22 H26 Co N4 O4 +, F6 P -'
_chemical_formula_sum            'C22 H26 Co F6 N4 O4 P'
_chemical_formula_weight         614.37
_chemical_name_systematic
'{2,2'-[<i>N</i>,<i>N</i>'-Bis(pyridin-2-ylmethyl)cyclohexane-<i>trans</i>-1,2-diyldi(nitrilo)]diacetato}cobalt(III) hexafluoridophosphate'
_space_group_crystal_system      orthorhombic
_space_group_IT_number           73
_space_group_name_Hall           '-I 2b 2c'
_space_group_name_H-M_alt        'I b c a'
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   13.9848(4)
_cell_length_b                   14.6221(4)
_cell_length_c                   22.2177(6)
_cell_measurement_reflns_used    9742
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.9967
_cell_measurement_theta_min      2.7246
_cell_volume                     4543.2(2)
_computing_cell_refinement
;
SAINT (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT (Bruker, 2008)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012)
;
_computing_publication_material
;
EnCIFer (Allen <i>et al.</i>,  2004) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type
;
Bruker APEXII diffractometer equipped with a CCD detector
;
_diffrn_measurement_method       '\f and \w'
_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  0.0167
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            57644
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.037
_diffrn_reflns_theta_min         1.833
_exptl_absorpt_coefficient_mu    0.917
_exptl_absorpt_correction_T_max  0.8336
_exptl_absorpt_correction_T_min  0.6906
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            'translucent dark red'
_exptl_crystal_density_diffrn    1.796
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelipiped
_exptl_crystal_F_000             2512
_exptl_crystal_size_max          0.436
_exptl_crystal_size_mid          0.356
_exptl_crystal_size_min          0.206
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.524
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         3630
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0287
_refine_ls_R_factor_gt           0.0270
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+5.6191P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0786
_reflns_number_gt                3401
_reflns_number_total             3630
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            zl2616sup1.cif
_cod_data_source_block           I
_cod_database_code               2240516
_cod_database_fobs_code          2240516
_shelx_estimated_absorpt_t_min   0.691
_shelx_estimated_absorpt_t_max   0.834
_shelx_hkl_checksum              31770
_shelx_res_checksum              12618