Crystal Structures, Gas Adsorption, and Electrochemical Properties of Electroactive Coordination Polymers Based on the Tetrathiafulvalene-Tetrabenzoate Ligand
Chen, Bin; Lv, Zhong-Peng; Leong, Chanel F.; Zhao, Yue; D’Alessandro, Deanna M.; Zuo, Jing-Lin; Crystal Growth & Design 15 (2015) 1861–; doi:10.1021/acs.cgd.5b00014

data_4512862
_publ_section_title
;
 Crystal Structures, Gas Adsorption, and Electrochemical Properties of
 Electroactive Coordination Polymers Based on the
 Tetrathiafulvalene-Tetrabenzoate Ligand
;
_journal_issue                   4
_journal_name_full               'Crystal Growth &amp; Design'
_journal_page_first              1861
_journal_paper_doi               10.1021/acs.cgd.5b00014
_journal_volume                  15
_journal_year                    2015
_chemical_formula_sum            'C39 H35 Ba N O12 S4'
_chemical_formula_weight         975.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           72
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2 2c'
_symmetry_space_group_name_H-M   'I b a m'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.4489(9)
_cell_length_b                   21.5552(19)
_cell_length_c                   38.344(3)
_cell_measurement_reflns_used    8306
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.41
_cell_volume                     8636.1(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1152
_diffrn_reflns_av_sigmaI/netI    0.0935
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            25896
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         1.89
_exptl_absorpt_coefficient_mu    1.173
_exptl_absorpt_correction_T_max  0.8079
_exptl_absorpt_correction_T_min  0.7349
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3936
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.19
_platon_squeeze_details
;
In order to subtract the contribution from the disordered solvent molecules,
the SQUEEZE command was applied.
SQUEEZE removed one DMF and one CH3CH2OH per formula unit. This valueis calculated based upon volume/count_electrons analysis.
See ref. Bi, Y. F.; Wang, X. T.; Liao, W. P.; Wang, X. F.; Wang, X. W.;
Zhang, H. J.; Gao, S. J. Am. Chem. Soc. 2009, 131, 11650.

CHEMW03_ALERT_2_A ALERT: The ratio of given/expected molecular weight as
            calculated from the _atom_site* data lies outside
            the range 0.90 <> 1.10
           From the CIF: _cell_formula_units_Z                    8
           From the CIF: _chemical_formula_weight           975.26
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   34.00  408.37
           H         1.01   22.00   22.18
           N        14.01    0.00    0.00
           O        16.00   10.00  159.99
           S        32.07    4.00  128.26
           Cl       35.45    0.00    0.00
           Ba      137.33    1.00  137.33
           Calculated formula weight              856.1
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for disordered DMF and CH3CH2OH omitted by SQUEEZE.
;
_refine_diff_density_max         2.868
_refine_diff_density_min         -1.764
_refine_diff_density_rms         0.232
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     223
_refine_ls_number_reflns         3857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.191
_refine_ls_R_factor_all          0.1043
_refine_ls_R_factor_gt           0.0952
_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^)+(0.0300P)^2^+200.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2258
_refine_ls_wR_factor_ref         0.2297
_reflns_number_gt                3165
_reflns_number_total             3857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5b00014_si_002.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'Ibam '
_cod_database_code               4512862