Crystal structure of bis[4'-(1,4,7,10-tetraoxa-13- azacyclopentadecan-13-yl)-2,2':6',2''-terpyridine]cobalt(III) tris(perchlorate) methanol monosolvate monohydrate
Ohmagari, Hitomi; Nakaya, Manabu; Ohtani, Ryo; Nakamura, Masaaki; Hayami, Shinya; Acta Crystallographica Section E 71 (2015) 997–999; doi:10.1107/S2056989015014164

data_2240981
_publ_section_title
;
 Crystal structure of bis[4'-(1,4,7,10-tetraoxa-13-
 azacyclopentadecan-13-yl)-2,2':6',2''-terpyridine]cobalt(III)
 tris(perchlorate) methanol monosolvate monohydrate
;
_journal_coeditor_code           IS5400
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              997
_journal_page_last               999
_journal_paper_doi               10.1107/S2056989015014164
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Co (C25 H30 N4 O4)2] (Cl O4)3, C H4 O, H2 O'
_chemical_formula_moiety         'C51 H66 Cl3 Co N8 O22'
_chemical_formula_sum            'C51 H66 Cl3 Co N8 O22'
_chemical_formula_weight         1308.42
_chemical_name_systematic
;Bis[4'-(1,4,7,10-tetraoxa-13-azacyclopentadecan-13-yl)-2,2':6',2''-terpyridine]cobalt(III)
tris(perchlorate) methanol monosolvate monohydrate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_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
_cell_angle_alpha                84.237(2)
_cell_angle_beta                 81.674(2)
_cell_angle_gamma                85.652(3)
_cell_formula_units_Z            1
_cell_length_a                   8.8080(8)
_cell_length_b                   9.5032(8)
_cell_length_c                   16.9321(14)
_cell_measurement_reflns_used    9503
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.47
_cell_measurement_theta_min      3.09
_cell_volume                     1392.6(2)
_computing_cell_refinement
;
<i>RAPID-AUTO</i> (Rigaku, 1995)
;
_computing_data_collection
;
<i>RAPID-AUTO</i> (Rigaku, 1995)
;
_computing_data_reduction
;
<i>RAPID-AUTO</i> (Rigaku, 1995)
;
_computing_molecular_graphics
;
CrystalStructure (Rigaku, 2014)
;
_computing_publication_material
;
CrystalStructure (Rigaku, 2014)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SIR2004 (Burla <i>et al.</i>,  2005)
;
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13693
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.481
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.370
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Rigaku, 1995)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             682.00
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.96
_refine_diff_density_min         -1.09
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 1715 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_parameters     774
_refine_ls_number_reflns         10375
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1362
_refine_ls_R_factor_gt           0.0856
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1411P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2146
_refine_ls_wR_factor_ref         0.2561
_reflns_number_gt                6395
_reflns_number_total             10375
_reflns_threshold_expression     F^2^>2\s(F^2^)
_cod_data_source_file            is5400sup1.cf
_cod_data_source_block           I
_cod_database_code               2240981
_cod_database_fobs_code          2240981