Valence Tautomeric Transitions of Three One-Dimensional Cobalt Complexes.
Chen, Xiang-Yi; Wei, Rong-Jia; Zheng, Lan-Sun; Tao, Jun; Inorganic chemistry  (2014) 141125084744006–; doi:10.1021/ic502471v

data_4341814
_publ_section_title
;
 Valence Tautomeric Transitions of Three One-Dimensional Cobalt Complexes.
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              141125084744006
_journal_paper_doi               10.1021/ic502471v
_journal_year                    2014
_chemical_formula_moiety         'C44 H52 Co N2 O4'
_chemical_formula_sum            'C44 H52 Co N2 O4'
_chemical_formula_weight         731.81
_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     iterative
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                100.843(5)
_cell_angle_beta                 99.057(8)
_cell_angle_gamma                100.687(7)
_cell_formula_units_Z            3
_cell_length_a                   15.2442(15)
_cell_length_b                   15.2808(8)
_cell_length_c                   16.9964(10)
_cell_measurement_reflns_used    4302
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      62.4190
_cell_measurement_theta_min      3.7400
_cell_volume                     3744.4(5)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'J. Appl. Cryst. (2007) 40, 786-790'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1139
_diffrn_reflns_av_unetI/netI     0.1340
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23567
_diffrn_reflns_theta_full        66.34
_diffrn_reflns_theta_max         66.34
_diffrn_reflns_theta_min         3.57
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.960
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.76754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.20 (release 27-06-2012 CrysAlis171 .NET)
(compiled Jul 11 2012,15:38:31)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            dark_green
_exptl_crystal_density_diffrn    0.974
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1167
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
Approximately 13.8% of the unit cell volume comprises a large region of
disordered solvent which could not be modeled as discrete atomic sites.
We employed PLATON SQUEEZE to calculate the contribution to the diffraction
from the solvent region and thereby produced a set of solvent-free diffraction
intensities. SQUEEZE estimated a total count of 175 electrons per unit cell.
According to the final formula which was calculated from TGA combined with 
elemental analysis data, these electrons were assigned to be 4 acetonitrile and 
4 water molecules per unit cell. 
;
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.169
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         12385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1485
_refine_ls_R_factor_gt           0.0944
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2372
_refine_ls_wR_factor_ref         0.2625
_reflns_number_gt                6219
_reflns_number_total             12385
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic502471v_si_002.cif
_cod_data_source_block           3Sat300K
_cod_database_code               4341814