Polymorphism of the dinuclear Co^III^–Schiff base complex [Co~2~(<i>o</i>-van-en)~3~]·4CH~3~CN (<i>o</i>-van-en is a salen-type ligand)
Vráblová, Anna; Černák, Juraj; Falvello, Larry R.; Tomás, Milagros; Acta Crystallographica Section C 75 (2019) 433–442; doi:10.1107/S2053229619003115

data_2021551
_publ_section_title
;
 Polymorphism of the dinuclear Co^III^--Schiff base complex
 [Co~2~(<i>o</i>-van-en)~3~]&#x00B7;4CH~3~CN (<i>o</i>-van-en is a
 salen-type ligand)
;
_journal_coeditor_code           KY3166
_journal_issue                   4
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              433
_journal_page_last               442
_journal_paper_doi               10.1107/S2053229619003115
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Co2 (C18 H18 N2 O4)3], 4C2 H3 N'
_chemical_formula_moiety         'C54 H54 Co2 N6 O12, 4(C2 H3 N)'
_chemical_formula_sum            'C62 H66 Co2 N10 O12'
_chemical_formula_weight         1261.10
_chemical_name_common
;[\m-Bis(3-methoxy-2-oxidobenzylidene)ethylenediamine]bis{[bis(3-methoxy-2-oxidobenzylidene)ethylenediamine]cobalt(III)} acetonitrile
tetrasolvate
;
_chemical_name_systematic
'{\m-6,6'-Dimethoxy-2,2'-[ethane-1,2-diylbis(nitrilomethylylidene)]diphenolato}bis({6,6'-dimethoxy-2,2'-[ethane-1,2-diylbis(nitrilomethylylidene)]diphenolato}cobalt(III)) acetonitrile tetrasolvate'
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_method           SHELXL-2018/1
_cell_angle_alpha                70.471(4)
_cell_angle_beta                 71.667(4)
_cell_angle_gamma                72.466(4)
_cell_formula_units_Z            1
_cell_length_a                   10.4971(5)
_cell_length_b                   11.6195(5)
_cell_length_c                   13.7158(6)
_cell_measurement_reflns_used    9604
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.6660
_cell_measurement_theta_min      3.5130
_cell_volume                     1460.26(12)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 1999) and Mercury (Macrae <i>et al.</i>,
2008)
;
_computing_publication_material
;
SHELXL2018 (Sheldrick, 2015b),
WinGX (Farrugia, 2012),
PARST (Nardelli, 1983),
Mercury (Macrae <i>et al.</i>,  2008) and
CrystalExplorer (Spackman & Jayatilaka, 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku Xcalibur Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0387
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20710
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.497
_diffrn_reflns_theta_min         3.245
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.641
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.83521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             658
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.144
_exptl_crystal_size_min          0.049
_refine_diff_density_max         0.889
_refine_diff_density_min         -0.348
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         6041
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0373
_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^)+(0.0446P)^2^+0.8220P] where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0941
_reflns_number_gt                5192
_reflns_number_total             6041
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ky3166sup1.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 2021550--2021551.cif.'
_cod_original_cell_volume        1460.26(13)
_cod_database_code               2021551
_cod_database_fobs_code          2021551
_shelx_estimated_absorpt_t_min   0.876
_shelx_estimated_absorpt_t_max   0.969
_shelx_hkl_checksum              32324
_shelx_res_checksum              43433