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_4512861
_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            'C43 H39 Cd N2 O13 S4'
_chemical_formula_weight         1032.40
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.313(5)
_cell_angle_beta                 79.259(6)
_cell_angle_gamma                86.749(5)
_cell_formula_units_Z            2
_cell_length_a                   9.005(3)
_cell_length_b                   12.573(4)
_cell_length_c                   19.675(7)
_cell_measurement_reflns_used    2561
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      2.51
_cell_volume                     2167.7(13)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.1012
_diffrn_reflns_av_sigmaI/netI    0.1315
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            12238
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    0.765
_exptl_absorpt_correction_T_max  0.8874
_exptl_absorpt_correction_T_min  0.8498
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1054
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
In order to subtract the contribution from the disordered solvent molecules,
the SQUEEZE command was applied.
SQUEEZE removed one DMF and three H2O 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                    2
           From the CIF: _chemical_formula_weight          1032.40
           TEST: Calculate formula weight from _atom_site_*
           atom     mass    num     sum
           C        12.01   40.00  480.44
           H         1.01   26.00   26.21
           Cd      112.41    1.00  112.41
           N        14.01    1.00   14.01
           O        16.00    9.00  143.99
           S        32.07    4.00  128.26
           Calculated formula weight              905.32
 
RESPONSE: This is caused by the given molecular weight being increased
from the atom count to account for disordered DMF and H2O omitted by SQUEEZE.
;
_refine_diff_density_max         0.745
_refine_diff_density_min         -1.634
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.903
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     497
_refine_ls_number_reflns         8011
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.903
_refine_ls_R_factor_all          0.0890
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1539
_refine_ls_wR_factor_ref         0.1650
_reflns_number_gt                4761
_reflns_number_total             8011
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            cg5b00014_si_002.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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      'P-1   '
_cod_database_code               4512861